222-00023J

Jul. 2016

Thermogravimetric Analyzer

TGA-50/50H

Instruction Manual
Read this manual thoroughly before you use the product.
Keep this manual for future reference.
This page is intentionally left blank.
Introduction
Read this Instruction Manual thoroughly before using
the product.
Thank you for purchasing this product.
This manual describes the installation, operation, hardware validation, usage cautions,
and accessories and options for this product. Read this manual thoroughly before using
the product and operate the product in accordance with the instructions in this manual.
Keep this manual for future reference.

Important
• If the user or usage location changes, ensure that this manual is always kept
together with the product.
• If this manual or a product warning label is lost or damaged, immediately contact
your Shimadzu representative to request a replacement.
• To ensure safe operation, read all "Safety Instructions" thoroughly before using
the product.
• To ensure safe operation, contact your Shimadzu representative if product
installation, adjustment, re-installation (after the product is moved), or repair is
required.

Notice
• Information in this manual is subject to change without notice and does not represent
a commitment on the part of the vendor.
• Any errors or omissions which may have occurred in this manual despite the utmost
care taken in its production will be corrected as soon as possible, although not
necessarily immediately after detection.
• All rights are reserved, including those to reproduce this manual or parts thereof in
any form without permission in writing from Shimadzu Corporation.

ã 1995-2016 Shimadzu Corporation. All rights reserved.

Original version is approved in English.

TGA-50/50H i
 Introduction

Safety Instructions
To ensure safe product operation, read these important safety instructions carefully
before use and follow all DANGER, WARNING and CAUTION instructions given in this
section.

1 Do NOT use the unit for the purpose other than the above mentioned analysis.

2 Follow the procedures described in the instruction manual.

3 Observe the warnings and cautions.

4 Do NOT disassemble or modify the unit without our approval.

5 For repair of the product inside, contact our sales office or agent.

Indications Used in This Manual

Dangers, Warnings, Cautions, and Notes are indicated using the following conventions:

Indication Meaning
Indicates an imminently hazardous situation which, if not
avoided, will result in serious injury or death.

Indicates a potentially hazardous situation which, if not

avoided, could result in serious injury or possibly death.

Indicates a potentially hazardous situation which, if not

avoided, may result in minor to moderate injury or equipment
damage.
Emphasizes additional information that is provided to ensure
the proper use of this product.

The following symbols are used in this manual:

Indication Meaning

Indicates an action that must not be performed.

Indicates an action that must be performed.

Indicates information provided to improve product performance.

Indicates the location of related reference information.

ii TGA-50/50H
 Warning Labels

Warning Labels
In order to ensure safety, warning labels are attached in places requiring caution.
If a warning label is lost or damaged, obtain a new label through your Shimadzu
representative and attach it in the correct position. See "Warning Labels on the
Equipment" in this Instruction Manual for details on the positions where the labels are
attached.

TGA-50/50H iii
 Introduction

Warranty
Shimadzu provides the following warranty for this product.

1. Period:
Please contact your Shimadzu representative for information about the period of this warranty.

2. Description:
If a product/part failure occurs for reasons attributable to Shimadzu during the warranty period,
Shimadzu will repair or replace the product/part free of charge. However, in the case of products
which are usually available on the market only for a short time, such as personal computers and
their peripherals/parts, Shimadzu may not be able to provide identical replacement products.

3. Limitation of Liability:
(1) In no event will Shimadzu be liable for any lost revenue, profit or data, or for special, indirect,
consequential, incidental or punitive damages, however caused regardless of the theory of
liability, arising out of or related to the use of or inability to use the product, even if Shimadzu
has been advised of the possibility of such damage.

(2) In no event will Shimadzu's liability to you, whether in contract, tort (including negligence), or
otherwise, exceed the amount you paid for the product.

4. Exceptions:
Failures caused by the following are excluded from the warranty, even if they occur during the
warranty period.

(1) Improper product handling

(2) Repairs or modifications performed by parties other than Shimadzu or Shimadzu designated
companies

(3) Product use in combination with hardware or software other than that designated by Shimadzu

(4) Computer viruses leading to device failures and damage to data and software, including the
product's basic software

(5) Power failures, including power outages and sudden voltage drops, leading to device failures
and damage to data and software, including the product's basic software

(6) Turning OFF the product without following the proper shutdown procedure leading to device
failures and damage to data and software, including the product's basic software

(7) Reasons unrelated to the product itself

(8) Product use in harsh environments, such as those subject to high temperatures or humidity levels,
corrosive gases, or strong vibrations

(9) Fires, earthquakes, or any other act of nature, contamination by radioactive or hazardous
substances, or any other force majeure event, including wars, riots, and crimes

(10) Product movement or transportation after installation

(11) Consumable items

Recording media such as CD-ROMs are considered consumable items.

* If there is a document such as a warranty provided with the product, or there is a separate contract
agreed upon that includes warranty conditions, the provisions of those documents shall apply.

iv TGA-50/50H
 After-Sales Service and Availability of Replacement Parts

After-Sales Service and Availability of Replacement Parts

n After-Sales Service

If any problem occurs with this product, perform an inspection and take appropriate
corrective action as described in "5 MAINTENANCE AND TROUBLESHOOTING" of this
manual.
If the problem persists, or the symptoms are not covered in "5 MAINTENANCE AND
TROUBLESHOOTING" ,contact your Shimadzu representative.

n Replacement Parts Availability

Replacement parts for this product will be available for a period of seven (7) years after
the product is discontinued. Thereafter, such parts may cease to be available.
Note, however, that the availability of parts not manufactured by Shimadzu shall be
determined by the relevant manufacturers.

Maintenance, Inspections, and Adjustment

In order to maintain the instrument's performance and obtain accurate measurement
data, daily inspection and periodic inspection/calibration are necessary.
• For daily maintenance, inspection, and replacement parts, see "5 MAINTENANCE AND
TROUBLESHOOTING" of this manual.
• Periodic inspection/calibration should be requested to your Shimadzu representative.
• Replacement cycles described for periodic replacement parts are a rough estimate.
Replacement may be required earlier than the described replacement cycles depending
on usage environment and frequency.

Disposal Precautions
When disposing of the instrument, contact your Shimadzu representative.
If you dispose them yourself, do so in accordance with the processing standards
determined by law, separately from general industrial waste and household garbage.

n For California, USA Only

This product contains a battery that contains perchlorate material.

Perchlorate Material - special handling may apply.
See www.dtsc.ca.gov/hazardouswaste/perchlorate

TGA-50/50H v
Contents
Introduction Safety Instructions .............................................. ii
Indications Used in This Manual ......................... ii
Warning Labels ................................................. iii
Warranty .......................................................... iv
After-Sales Service and Availability of
Replacement Parts ............................................. v
Maintenance, Inspections, and Adjustment ........... v
Disposal Precautions ........................................... v

1 INSTALLATION 1.1 Detailed Contents ................................................ 1

1.2 Requirements and Precautions for Installation ....... 2
1.3 Installation .......................................................... 3
1.3.1 Electrical section ................................................ 4
1.3.2 Purge gas ....................................................... 5
1.4 Cable Connection with Data Saving Equipment
........................................................................... 6
1.4.1 TA-60WS System ................................................ 6

1.4.2 Analogue Recorder .............................................. 7

1.5 Inspection and Adjustment ................................... 7

2 SPECIFICATIONS

PRINCIPLE AND 11
3 STRUCTURE
3.1 Outline .............................................................

3.2 Principle ........................................................... 11

OPERATIONS FOR 4.1 Basic Operation (example measurement of

4 MEASUREMENT copper sulfate dehydration) ............................... 13
4.2 Technique of Analysis ........................................ 16
4.2.1 Sample and sample cell ...................................... 16
4.2.2 Setting of atmosphere ........................................ 17

vi TGA-50/50H
 Contents

4.2.3 Moving the furnace up and down ........................... 20

4.3 Precautions for Measurement ............................. 21

MAINTENANCE AND 22
5 TROUBLESHOOTING
5.1 Installation of suspention wire ...........................

5.2 Troubleshooting ................................................ 22

5.3 Consumable parts .............................................. 25
5.4 Preservation ...................................................... 25

(APPENDIX)Detailed 26
6 Explanation of keys
6.1 Operations for measurement ..............................

6.1.1 Start of measurement ......................................... 26

6.1.2 End of measurement .......................................... 26

6.1.3 Forced termination of measurement .......................... 26

6.2 Normal display .................................................. 27

6.3 Explanation of keys ........................................... 27
6.4 Temperature Program ........................................ 29
6.5 AUTO ZERO ...................................................... 34
6.6 TIME SCALE ...................................................... 34
6.7 POWER KEEP/OFF(power off) .............................. 36
6.8 PID（PIO constants for temperature control) ........ 37
6.9 FILE DELETE（File deletion） .............................. 38
6.10 FILE SAVE（File saving） .................................... 39
6.11 FILE LOAD（(File call) ......................................... 40
6.12 CALIBRATION（Calibration) ................................. 40
6.13 RANGE（Weight signal range） .......................... 42
6.14 Error messages .................................................. 43

TGA-50/50H vii
This page is intentionally left blank.
1 INSTALLATION
The TGA-50 is shipped under the particulars given in section "1.1 Detailed Contents"
Check the quantity of each part according to the contents detailed in section "1.1 1
Detailed Contents" . If any shortage of parts or damage from transportation is found,
please contact the forwarding agent and Shimadzu.

1.1 Detailed Contents

Quantity
Part name Part No.
M type H type
Main unit for 120V AC or Main unit for
1 1
220/240V AC*1
Balance mechanism unit 1 1
Connecting section 1 1
Furnace unit (middle temperature type) 222-01216-91 1 0
Furnace unit (high temperature type) 222-01216-92 0 1
Standard accessories
Suspension wire (nichrome) 35mm 201-53157-03 1 1
Suspension wire (quartz) 155mm 201-55162-03 2 2
Suspension wire (platinum) 155mm 201-52684-06 0 1
Sample cell (Pt Rh) 201-51976 1 1
Sample pan (Pt) 201-52686-01 1 1
Weight pan 201-52693-01 1 1
Weight set 201-52724-01 1 1
O-ring P8 *2 036-10206 3 3

O-ring P22 *2 036-11022 3 3

O-ring P25 *2 036-10226 3 3

O-ring 4CSS-022 *2 670-11509 3 3

Joint set, glass column 221-15561-91 1 1
Graphite ferrule 221-15563-91 1 1
Cap (reaction tube bottom) 222-01393 1 1
Silicone packing 201-35184 1 1
Pipe 222-01690-91 1 1
Nut MF *1 201-30008 1 1

Nipple MNO *1 201-30009 1 1

Washer WM *1 201-30051 1 1
Tweezers 086-16103-01 1 1
Wrench HX 086-03804 1 1
Instruction manual (this manual) 222-00022 1 1

TGA-50/50H 1
 1 INSTALLATION

*1 The B-20 step-down transformer (670-17491), packaged separately, is attached as a standard

accessory.
*2 If you wish to order, add -84 after the parts number. Each set includes 5pcs.
*3 If you wish to order, add -84 after the parts number. Each set includes 10pcs.

1.2 Requirements and Precautions for Installation

• The power supply should be 110V ~ 130V or 200V ~ 260V AC, 50/60 Hz
TGA-50H (high temperature type) : 1200VA
TGA-50M (middle temperature type) : 1000VA

Where the power supply has a continuous voltage fluctuation of 2V or more, a

stabilizer may be required.

• Use a dedicated stand (table) to reduce the effects of vibration as much as possible.
However, for measurement in the range of ± 200 mg, the instrument may be installed
together with a recorder and others on a solid lab table.
• For safety and stable measurement, connect the power supply plug of the TGA-50 main
body or the B-20 step-down transformer to a socket-outlet with earthing
contact(s);otherwise use an adapter plug with earthing contact(s) which should be
grounded.
• Avoid installing the instrument at a place exposed to direct sunlight or near the
outlet of an air-conditioner.
• Operate the instrument at a room temperature not less than 5°C and not more than
40°C and a humidity of 80% or less.

• Recommending data processor is a system which consists of a personal computer and

a program which has been supplied by SHIMADZU. Please refer to an instruction manual
to know how to operate the system.

2 TGA-50/50H
 1.3 Installation

• "Fig.1-1","Fig.1-2"show the outside dimensions and outline of the instrument.

Fig.1-1

1.3 Installation
The name of each section is shown in "Fig.1-2".

Fig.1-2

TGA-50/50H 3
 1 INSTALLATION

1.3.1 Electrical section

Connect the power supply plug of the TGA-50 main body directly to a socket-outlet with
earthing contact(s) of 120VAC, or connect it first to one of the socket-outlet of the B-20
step-down transformer and second connect the power supply plug of the B-20 to a
socket-outlet with earthing contact(s) of 220/240 VAC.
"Fig. 1-3 Power Supply Connection"

If any socket-outlets with earthing contact(s) are not available, use an adapter plug with
earthing contact(s) which should securely grounded.

To avoid electric shock, supply electric power from a socket-outlets with

earthing contact(s); otherwise use an adapter plug with earthing contact(s)
which should be grounded.

In the case of 120 VAC power supply...

In the case of 220/240 VAC power supply...

4 TGA-50/50H
 1.3 Installation

Fig. 1-3 Power Supply Connection

Fig. 1-4 B-20 Step-down Transformer

1.3.2 Purge gas

1 Connect the "GAS INLET" joint at the lower part of the rear panel to the gas
cylinder.

2 Adjust the cylinder outlet pressure to 0.6-1.0 MPa.

3 Set the gas flow rate by the adjusting knob while observing the gas flow meter
on the left side(facing the front) of the TG section.
The indicator shows the flow of nitrogen gas in mL/min.
When the knob is turned clockwise, the flows increases. When the knob is turned
counterclockwise, the flows reduced.

TGA-50/50H 5
 1 INSTALLATION

1.4 Cable Connection with Data Saving Equipment

1.4.1 TA-60WS System

In Shimadzu TA-60WS thermal analysis system, a single personal computer (for general
use, of IBM PC/AT compatible types or 286 PS/2 Model 30 series) manages up to four 50
series thermal analysis modules such as TGA-50. The whole system configuration is shown
in"Fig. 1-5 TA-60WS system configuration". For detailed information, refer to the
instruction manual of the TA-60WS.

Fig. 1-5 TA-60WS system configuration

Connection between the TGA-50 and the TA-60WS interface should be carried out as
follows. Connect "RS-232C" connector on the rear panel of the TGA-50 and one of "CH1"
~ "CH4" connectors on the rear panel of the TA-60WS interface with the transmission
cable (supplied with the TA-60WS, about 3m long).
"Fig. 1-6 Connection with TA-60WS"

2nd to 4th TGA-50's are to be connected to unoccupied "CH XX" connectors of the
TA-60WS interface.

Fig. 1-6 Connection with TA-60WS

6 TGA-50/50H
 1.5 Inspection and Adjustment

1.4.2 Analogue Recorder

All the 50 series thermal analysis modules have analog signal output so that they can be
connected with connectional pen-recorders for obtaining analog data charts. 1
In case of analog signal recording, an optional accessory kit listed below is necessary.

Part Name Part Number Q'ty

Analog signal cable 222-13134-41 1
Recorder cable 222-01672-91 1
Terminal block for recorder 222-01670-91 1

For example, connection with Shimadzu R-122TP two-pen recorder is as follows.

Connect the analog signal cable between "RECORDER" connector on the right side panel
(viewed from the front) of the electrical section of the TGA-50 and the connector on the
terminal block. Connect the recorder cable between the terminal block and the R-122TP
as shown in "Fig. 1-7 Connection of Recorder".

Fig. 1-7 Connection of Recorder

If the recorder power cable is plugged into the service outlet in the TGA-50 rear panel,
recorder power can be turned off automatically.

1.5 Inspection and Adjustment

After installing the instrument according to section "1.3 Installation", check to see if it
operates normally.

1 Turn on the power switch on the main unit and wait for 5 minutes or so.

2 If the furnace is positioned upward, press the[q]key to move it downward. In this

case, remove the weight cover beforehand.

3 Turn the BALANCE knob to cause the weight signal to come near zero. If the
weight signal does not come near zero, put an appropriate weight on the sample
pan or weight pan to move it near zero.

TGA-50/50H 7
 1 INSTALLATION

4 Adjust the position of the point of the thermocouple. As shown in "Fig. 1-8
Adjustment of Thermocouple Position", a point about 3-4 mm just under the
sample pan is optimum. Do not bring both into contact with each other.

5 Press the[p] key to move the furnace unit upward. Set the weight cover.

Fig. 1-8 Adjustment of Thermocouple Position

6 Let purge gas flow. An appropriate flow rate is about 10ml/min. In this condition,
check each item in the following table.

Cause of abnormality and

Check item
countermeasure
If "Acquisition : Status" window
Does the liquid crystal display on the
doesn't appear on the PC monitor,
panel show the TG monitor?
please contact our service staff.
Does the temperature indicator indicate Check to see if the sensitive point of
a value of room temperature ±3°C that the thermocouple is not in contact with
time? the sample pan or others. If the
Is the temperature indicator stable countermeasure is ineffective, please
around a central value ± 0.2 °C? contact our service staff.

Check that the suspension wire, sample

pan and weight pan are not in contact
with the internal wall of the furnace
and weight cover. If the instrument is
not perpendicular， turn the height
Is the change of weight indicator
adjusting screws to change its
stabilized at ±0.001mg or so?
inclination so that the suspension wire
is in the center of the purge gas pipe.
Check that there is no source of
vibration near the instrument and that
the feet are positioned properly.

8 TGA-50/50H
 1.5 Inspection and Adjustment

7 Next, press the [START]key to put the instrument into the "MEASURE" status.
(The "MEASURE" lamp on the flont panel comes on.)
At this time, check the following items.

Cause of abnormality and

1
Check item
countermeasure
Does the temperature indication
change?
(After [START],the temperature rises If the temperature won't change or it
about 5°C in 30 seconds.) begins to fall, please contact our
service staff.
Is the change in temperature indication
upward?

If all the above items are found normal, the installation is satisfactory. Press the[STOP]
key to complete the measurement. The instrument goes from the "MEASURE" status to
the "READY" status.

The "READY" lamp on the front panel comes on. If the furnace temperature
rises above 40°C, the "READY" lamp blinks.

When the instrument is not going to be used immediately after completion of inspection,
move the furnace unit to its upper position for protection so that the sample pan is not
exposed.

Whenever the instrument is not used henceforth, be sure to put the

furnace unit in this position.

TGA-50/50H 9
 2 SPECIFICATIONS
Balance type Taut band
Temperature range Middle temp. type : Room temperature to1000℃
(Thermocouple used :Chromel-alumel)
High temp. type : Room temperature to 1,500°C
(Thermocoup1e used : Platinum - Platinum rhodium 10%)
Sample volume 1 gram including tare
Atmosphere Air, inert gas, gas stream and vacuum (Max. vacuum
achievable : 0.13Pa)
Dimensions 173mm(W) (adjusting foot 245 mm) ´ 550 mm(D) ´ 500mm(H)
Weight Approx 23kg
Readability 0.001mg
Measuring range ±20mg, ±200mg and "AUTO"

Balance adjusting range A range equivalent to ± 50mg

Rated output 1mg/mV(measuring range ± 20 mg),
10mg/mV(measuring range ± 200 mg)
Differential output 1mg/min/mV(measuring range ± 20 mg),
10mg/min/mV(measuring range ± 200 mg)

Measurement accuracy ± 1% of each range

Current requirement M type :1000VA, H type:1200VA

10 TGA-50/50H
3 PRINCIPLE AND STRUCTURE
3.1 Outline
This is a high-performance thermogravimetric analyzer having high sensitivity, high
vibration resistance and a structure that permits easy replacement of sample atmosphere.
The instrument is optimally applicable to the measurement of adsorbed water, water of
crystallization and studies of the thermal stability of substances and decomposition and
oxidation reactions from solid (liquid) to gas and gas to solid (liquid).

3.2 Principle
3

Fig.3-1 System Block Diagram

Usually, a sample is put in a platinum sample cell and then this cell is put on the sample
pan hanging down in the reaction tube where the atmosphere can be controlled.
Weights equivalent to the sample are put on the weight pan to almost balance the beam.

TGA-50/50H 11
 3 PRINCIPLE AND STRUCTURE

When the weight of the sample is changed by heating the sample, the beam supported
by the taut band inclines. This inclination is detected by the photoelectric elements and
then amplified. A current flows to the feedback coil to provide a uniform magnetic field
to balance with the moment of rotation based on the mass change of the sample. In
this way, the beam position is kept at a fixed position (zero-position method). At this
time, as the torque is in direct proportion to the current, mass changes of the sample
can be measured continuously with accuracy by sampling this current and recording it.

12 TGA-50/50H
4 OPERATIONS FOR MEASUREMENT
4.1 Basic Operation (example measurement of copper sulfate dehydration)

n Startup of the system

First, turn on the power switches of the TGA-50, the TA-60WS, the personal computer,
the display (if necessary), the printer, etc. After "TA Main Menu" appears on the display,
double-click "Acquisition : Status" icon, and select the channel (CH1 ~ CH4) where the
TGA-50 is connected. Now the frame is for monitoring the TGA-50 status. Check if there
are any anomaious indications for numerical or graphical values of time, temperature, or
TG signal. If so, take appropriate measures according to the respective instructions.

n Setting the sample

To avoid finger pinch, keep hands off the moving furnace.

4

1 Depress[q] key to lower the furnace unit.

2 Swing the cell support plate under the pan and put the clean empty sample cell
on the sample pan.
After this, swing the cell support plate back to the rest position.

3 Depress [p] key to raise the furnace unit.

4 Let nitrogen flow at a rate of 50 to 100mL/min.

"4.2.2 Setting of atmosphere"

5 Turn the (balance) knob on the front panel so that the 2 LEDs in the center of
the LEVEL meter come on.

6 Adjust the value of TG with [AUTO ZERO] key.

Operation Indication on liquid crystal display after operation

[AUTOZWRO]

TGA-50/50H 13
 4 OPERATIONS FOR MEASUREMENT

Operation Indication on liquid crystal display after operation

[ENT]

7 Depress[q] key to lower the furnace unit.

8 Swing the cell support plate under the pan, and fill the sample with copper
sulfate up to 1/3 of the capacity. Put this sample again on the sample pan and
swing the cell support plate to the rest position.

9 Depress [p] key to raise the furnace unit.

14 TGA-50/50H
 4.1 Basic Operation (example measurement of copper sulfate dehydration)

n Inputting of the measurement conditions

1 With the TA-60WS frame for monitoring the TGA-50 connected channel, open
the "Information window, input for necessary items (the file name, the sample
name, the sample weight, etc.), and finally click the "OK" button.

2 Open the "Parameters" window and setting the operating conditions as follows
before closing it.
• Sampling parameters
Sampling time: [ 1.0 ] [sec]
• TEMP program

Rate[°C/min] Hold temp[°C] Hold time[min]

1 15.0 350.0 0
2 0.0 0.0 0

4
This temperature program is as shown in the figure below.

n Measurement start

1 Click the "Start" button after check of lighting "READY" LED on the front panel
of the TGA-50.

2 The channel temp. indicating bar changes its color to pink, and "READY"LED go
off and "MEASURE"LED lights. Data acquisition now begins.

Avoid touching the furnace when at higher temperatures.

TGA-50/50H 15
 4 OPERATIONS FOR MEASUREMENT

n Measurement End

1 When the temperature reaches 350°C,i.e., the preset "Hold Temp".

Data acquisition is terminated and the data file is generated. The channel temp indicating
bar becomes blue after the several second sky blue period.

If POWER OFF is preset by the [FUNC]key, the power supply of the TGA is turned
off automatically.

n Data Analysis

Most principal aim of TG analysis is to obtain the weight loss or gain of the samples.

1 Make "Acquisition : Status" window to an icon, and double-click "Analysis"icon

in the "TA Main Menu" window.

2 Select the data file of just previous measurement in the file name table. If the
displayed table is not for the directory where the previous measurement file is
stored, change the directory.
Make use of "Preview" function (file searching with additional informations such as
"Graphic Display") or "Search" function (file selection referring to a preset key word such
as a certain sample name), if necessary. After the file to be analyzed from now is found,
double-click the file name (displayed with white letters) to open the file.

3 Data curve(s) is/are displayed with auto-scaling (for both abscissa and ordinate).
Change the display setting (such as abscissa choice between time/temp., ordinate choice
between absolute/normalized weight change, or the line style and color), as well as the
display region (i.e, zooming up/down), if necessary.

4 Select "Weight loss analysis" item in the pull-down "Analysis" menu. Use the
mouse to specify two points along the weight change curve. The weight loss
(%) and/or weight loss (mg) between the two specified points will be displayed.
Weight loss (% units) cannot be found for data for which no sample weight input.

5 If all jobs have finished, click the "Exit" key to retrieve initial display.

6 Select "Report" window and click the "Print" key, the results of analysis will be
printed.

4.2 Technique of Analysis

4.2.1 Sample and sample cell

16 TGA-50/50H
 4.2 Technique of Analysis

A powder sample or a sample to be melted by heating is put in the supplied platinum

cell for measurement. If the sample may react with platinum, use a ceramic cell or quartz
cell.

In an atmosphere without oxygen at a temperature of 5000C or less, and

aluminum cell can be used. For a flat, solid sample which will not melt (e.g.,
metal), a hole may be made in the sample and this may be hung directly on
the supension wire hook for measurement, without using the sample pan or
sample cell. In this case, the limit of sample weight is 1 g.

4.2.2 Setting of atmosphere

Thermogravimetry always has a connection with the gas phase. Therefore, if the sample
is measured in a fixed atmosphere flow constantly around it to prevent a rise or drop
of partial pressure, better data reproducibility will be obtained and data analysis will be
easier. The measurement in a static atmosphere is suitable for special purposes because
there occur changes in partial pressure. An oxidizing atmosphere, inert gas, reducing
atmosphere, corrosive gas, gas containing vapor,etc. are applicable as required. The
TGA-50 is provided with 4 gas ports to facilitate these measurements.
4
"Fig.4-1 Location of TGA-50 Gas Flow Ports"

When the evolved gas is noxious or poisonous, do not discharge it directly,

but use a trap or operate in the hood.

The type of atmospheric gas used and the standard flow rate in the TGA-50/50H are as
follows.

(I) : Nitrogen, helium, argon, etc. 50 to 100 mL/min

(II) : Air and oxygen 10 to 30 mL/min

When nitrogen or another inert gas is used as the atmospheric gas, for measurements
in which reaction of the sample with oxygen in the air is to be avoided, prior to
measurement, sufficiently replace the gas by supplying the gas at a flow rate of 100
mL/min for 30 minutes or more, and then start the measurements with 100 mL/min in
order to prevent reaction between the sample and oxygen. (Increasing the flow rate to
50 to 100 mL/min increases the oxidation prevention effect, but the amount of drift also
increases as described below. For samples with comparatively slow oxidation reaction
rates, to reduce the amount of drift, perform the measurements at 50 mL/min.)
Note that with this instrument, the baseline drift increases as the flow rate is increased,
so it is recommended that a blank measurement result (measurement in a blank cell) is
deducted from the sample measurement result (blank measurement). The blank correction
after measurement allows the change of the sample weight associated with
thermogravimetry to be accurately measured. Also, instead of passing the atmospheric
gas for 30 minutes in advance, gas can be replaced using a vacuum pump. However in

TGA-50/50H 17
 4 OPERATIONS FOR MEASUREMENT

order to prevent leakage of oxygen, select 50 to 100 mL/min as the gas flow rate during
measurement.

n Blank Correction

The change of the sample weight associated with thermogravimetry can be more
accurately obtained by applying the blank correction to the baseline drift caused by the
change in buoyancy.

Blank correction procedure

1 Blank data measurement

Measure an empty sample cell under the same conditions as the sample
measurement (heating rate, atmospheric gas type and flow rate, and type of
sample cell).

2 Sample data measurement

Measure the sample.

3 Blank correction
・Read the sample data into a TA60 window.
・Selecting the data curve to be corrected with a mouse displays a mark that
indicates that the curve has been selected.
・Select the [Manipulate]-[Baseline Correction [Blank]] command to open the
[Baseline Correction [Blank]] dialog box. Select the previously measured blank data
as the blank data file name, and select [Adjust Time] as the correction method.
Click the [OK] button to perform the blank correction.
After the blank correction, there is a slight increase in noise on the sample data. In order
to prevent this, perform a smoothing operation on the blank data with about 30 or
more points, and use the stored data as the blank data.

Fig.4-1 Location of TGA-50 Gas Flow Ports

Purge of the gas generated from the sample

Close gas ports ② and ④, and introduce gas from port ① and discharge it from port ③.

18 TGA-50/50H
 4.2 Technique of Analysis

As purge gas, flow a mixed gas of air or oxygen and nitrogen for an oxidizing
atmosphere, or flow nitrogen gas for an inert atmosphere. The gas is discharged from
port ③ after passing around the sample.

Measurement in reactive gas

To measure in a reactive gas (e.g., corrosive gas or moisture), introduce purge gas (air
or nitrogen gas) from port ①, and introduce the reactive gas from port ②, and discharge
it from port ③.
In this case, the purge gas flow can be several ml/min.
When measuring in a corrosive gas stream, be sure to allow flow of purge gas so as to
prevent the corrosive gas from entering the balance mechanism both during and after
measurement.

Gas substitution
For such a sample as is liable to react with oxygen, inert gas is used as atmospheric gas.
However, if the atmosphere is not completely substituted for the inert gas, it may react
sample with oxygen, which remains in a very small quantity, making the most suitable
analysis impossible.
In this case, close ports ② and ③, inert gas is filled up around the sample from port ①
after with vacuum pump connected port ④ of balance case of this equipment, exhausting
gradually for air inside furnace and balance unit. 4
Repeating this operation three to five times enables the oxygen partial pressure to be
reduced in the atmosphere around the sample.

To perform this operation, attach a pinch cock to the vacuum hose to adjust
the exhaust gas flow rate.
* If the vacuum pump rapidly discharges the gas,the balance unit may be damaged.

When filing the vacuum pan with inert gas starting with reduced pressure, it is necessary
to know whether the internal pressure has returned to the atmospheric pressure. There
is a simple way to know this. Connect a balloon to the gas outlet located at the upper
part of the furnace. When the balloon etc. which is deflated due to reduced pressure
has been inflated, the inside of the vacuum pan goes back to the atmosphere pressure.
When filing the vacuum pan with inert gas, stopping the vacuum pump can cause the
oil to backflow, resulting in a failure. The vacuum hose is pinched with the pinch cock,
and the vacuum pan fills with inert gas without stopping the vacuum pump.
The use of the special attachments VAC-50 Gas Evacuator (346-65331-91) allows
monitoring the pressure. The gas can be exhausted or changed easily by using the stop
valves located on the panel, which are related to the exhaust and pressure reducing lines.
When the port ① is closed, nipple MNO, washer WM and nut MF are used, and when
the port ③ is closed joint set (glass column), graphite ferrule and cap are used.
"Fig.4-2"

TGA-50/50H 19
 4 OPERATIONS FOR MEASUREMENT

If the sample evolves a harmful or toxic gas, do not discharge the gas directly
into the air.
Take an appropriate treatment for the exhaust gas, before discharging the gas
into the air.

Fig.4-2

4.2.3 Moving the furnace up and down

During measurement The furnace unit can not be moved down.

Ready for measurement at
When both the [q] key and [ENT] key are pressed at the same
a furnace temperature of
time, the furnace unit can be moved down.
40°C or more.

Ready for measurement at

When the [q] key is pressed once, the furnace unit can be
a furnace temperature
moved down.
less than 40°C.

• Regard the sample temperature as equal to the temperature displayed on the

liquid
crystal display.
• To move the furnace unit up, press the [p] key once.
• To stop the movement of the furnace unit halfway, press the [STOP] key. When
the [p] key or [q] key is pressed again, the furnace unit continues to move
up or down.

20 TGA-50/50H
 4.3 Precautions for Measurement

When the temperature of the furnace is 500 °C or more, do not turn off the
power supply of the TGA-50 main unit.
This may damage the O-ring.

After measurement in a reactive gas, stop the gas before moving the furnace
down.

4.3 Precautions for Measurement

1 The high sensitivity TGA-50 thermogravimetric analyzer must be handled with

special care.Before starting measurement, the suspension wires, sample pan and
sample cell must be made clean. If they are touched directly with fingers, sweat
4
and stains adhere, thereby causing serious measurement errors.

2 For the balance mechanism, precise leveling is not always required. However, the
perpendicularity of the reaction tube, suspension wire, sensitive point of the
thermocouple, suspension wire on the weight pan side and weight cover need
care ; be careful not to bring them into contact with one another.

3 For high-sensitivity measurement, a more stable measurement is gotten if the unit

is started at least 30 minutes after the power supply is turned on.

4 When the suspension wires and sample pan vibrate, noise will be included in the
recording. After they become completely still, still, start measurement. If the
vibration can not be stopped, turn the power supply off and check to see if any
external vibration is acting on the TGA-50.

5 Atmospheric gas must be controlled carefully according to the purpose of

measurement.
Where corrosive gas is used, do not forget the purge gas.

6 If the purge gas flow from port ① becomes large, the drift becomes larger as the
temperature rises. For a large purge gas f1ow, use port ②. In this case, port ① is
closed by nipple MNO and connect by the pipe in the accessories from port ② to
purge gas outlet.

TGA-50/50H 21
 5 MAINTENANCE AND TROUBLESHOOTING
5.1 Installation of suspention wire
Remove the weight cover on the lower
rear side of the balance mechanism unit
base and set the weight suspention wire
(35 mm long) and weight pan. Hook the
suspention wire on the ring located at the
lower end of the hook on the beam.
Set the 155 mm quartz suspention wire (Pt
for the high temperature type) as a
suspention wire on the sample side,and
install the sample pan.
Fig. 5-1

5.2 Troubleshooting

Symptom Possible cause Remedy

The temperature indication Defective connection of the
Retry connection.
isabnormal. thermocouple
(It does not become stable at
room temperature.) Broken thermocouple wire Replace the thermocouple.

After [START], the The fuse has blown Replace the fuse.
temperature does not rise.
("HEATER FAILURE" is Broken heater wire Replace the furnace unit.
displayed.)
The balance is not in
Readjust the balance.
equilibrium.
The weight signal is excessive. The lamp (6.3V) for
photoelectric elements has Replace the lamp.
burnt out.
The suspension wire or
sample pan is in contact
Check and make
with the reaction tube,
readjustment.
weight cover or
thermocouple.
Remove the source of
External vibration
vibration.
The noise of the weight
signal is large. The instrument is directly Install the instrument in
exposed to a strong draft. another place.
Remove the noise source or
There is an electrical noise
install the instrument in
source near the instrument.
another place.
The power supply condition Supply power through a
is bad. power stabilizer

22 TGA-50/50H
 5.2 Troubleshooting

Symptom Possible cause Remedy

The temperature control
constants (PID) are not Charge the control constant.
proper.
The temperature of the
The point of the
sample deviates markedly
thermocouple is in contact Readjust the thermocouple
from the program
with the furnace core tube position.
temperature. (Defective
or sample pan.
temperature control)
Remove the noise source or
There is an electrical noise
install the instrument in
source near the instrument.
another place.
Tle suspension wire or
sample pan is in contact
Check and make
with the reaction tube,
The TG cuerve has no readjustment.
weight cover or
reproducibility. thermocouple.
Defective gas purge Check the piping and seals.
(clogging, leakage, etc.) Replace parts.
An extra increment or
The suspension wire, sample Clean with acetone or
decrement appears on the TG
pan or sample cell is stained. replace with new ones.
curve.
The temperature of the
Check the wiring of the
balance mechanism has been
cooling fan, replace the
increased due to a failure of
Excessive drift can be seen on the cooling fan. cooling fan.
the TG curve.
The purge gas flow is too
Check the purge gas flow. 5
(Reduce it to 50mr/min or
large.
less.)
The fixing screws for shields
Check the furnace unit or
When the furnace moves up are loose or have gotten out
reassemble it.
and down, and unusual sound of place.
is heard. The reaction tube is
Replace the furnace unit.
damaged.
The furnace unit is installed Readjust the installation
in an lmproper position. position.
The movement of the furnace
is abnormal. Readjust the position of the
The top or bottom detector
(Movement is impossible. The detector or replace the point
or shutter is defective.
furnace does not stop at the detector.
top point or bottom point. Or The rack and pinion gear are Readjust the positional
the reaction tube hits against not engaged. relation.
the radiator fins.)
The motor or relays are Check the wiring or replace
defective. parts.

TGA-50/50H 23
 5 MAINTENANCE AND TROUBLESHOOTING

Symptom Possible cause Remedy

Turn the power supply off
The CPU is out of control.
and then on.*1
The temperature of the
liquid crystal has gone up
Check the wiring of the
because the cooling fan in
cooling fan or replace the
the lower part of the
cooling fan.
heating furnace unit is
The liquid crystal display is defective.
abnormal.
The liquid crystal display unit Replace the liquid crystal
itself is defective. display unit.
Tum the power supply off
and then on while
Backup of RAM is not
both[p]key and [q] key
normal.
are pressed at the same time.
(RAM initialization)
Key operations can not be Turn the power supply off
The CPU is a runaway.
accepted. and then on.*1

*1 Turn the power supply on while both [p] key and [q] key are pressed at the same time.

In the case of any troubles other than those with a background color, our
service staff shall take remedial measures. So please contact us. Please
understand that Shimadzu will not take responsibility for any deterioration of
system performance or safety resulting from breaking up or revamping the
instruments at your own discretion.

To avoid electric shock, replace the fuse after turning off the power switch
and disconnect the power supply plug from the socket-outlet.

24 TGA-50/50H
 5.3 Consumable parts

5.3 Consumable parts

Part Name Part Number Remarks

Furnace (middle temperature type reaction tube) 222-01227-91
Furnace (high temperature type reaction tube) 222-01225-91
Thermocouple C-A 222-01292-91
Thermocouple P-R 222-01292-93
Sample suspension wire (quartz) L=155 201-55162-03
Sample suspension wire (Pt) L=155 201-52684-06
Suspension wire (Nichrome) L=35 201-53157-03
O-ring P22 036-11022-84 for reaction tube, 5PCS
O-ring 4C SS-022 670-11509-84 for reaction tube, 5PCS
Graphite ferrule 4 pices 221-15563-91
Sample cell Pt 201-51976
Sample panl Pt 201-52686-01
Al crimp cell (50 pieces) 6f´2.5 mm 201-52943
Ceramic cell 6f´2.5 mm 201-54321
Quartz cell 6f´2.5 mm 201-54439
Pt cell (semi-macro) 6f´5 mm 201-53843
A Pt sample cell is provided as the standard sample cell. However, as for the ceramics
cell and the quartz cell as well, it is being made as mentioned above. 5

5.4 Preservation
When the instrument is not to be operated for a long time, remove the suspension wires
and pan and clamp the balance beam. Then, put the furnace unit in the raised position.
Close the gas ports with nipples and nuts. Do not tilt the instrument or stand it upside
down. Do not store the instrument in a place which is exposed to direct sunlight and
strong vibration, or a place which is full of dust. Put the removed suspension wires and
pans in the accessory case together with the other accessories for the next use.

TGA-50/50H 25
 6 (APPENDIX)Detailed Explanation of keys
6.1 Operations for measurement

6.1.1 Start of measurement

Check that the [READY] lamp lights and press the [START] key.

When the [READY] lamp is off, measurement can not be started even if the
[START] key is pressed.

After the [START] key is pressed, the [READY]lamp goes out. If the furnace is in the down
position, it will automatically go up.
When the heating furnace has gone up, the [MEASURE]lamp comes on and the
temperature of the sample begins to rise or fall according to the preset program.

6.1.2 End of measurement

When the temperature program terminates, the power supply of the heater is turned
off and the MEASURE lamp goes out.
If POWER OFF is preset, the power supply of the recorder and power supply of the
furnace are tumed off and all the display on the panel disappears when the temperature
of the sample section falls below 500°C.

To restart measurement, turn off the main switch and then turn it on again.
After recovery from a power failure, the power supply of the recorder will be
turned on and the display will reappear. However, the power supply of the
furnace will no be tumed on.

6.1.3 Forced termination of measurement

By pressing the [STOP] key during measurement, the measurement can be terminated
forcedly at that moment.
When the [STOP] key is pressed, the power supply of the heater is turned off.
However, when measurement has been terminated by pressing the [STOP] key, the power
supply of the recorder is not turned off even if POWER OFF is preset.

26 TGA-50/50H
 6.2 Normal display

6.2 Normal display

Except during setting, the following items are displayed.

n Current sample temperature

The temperature of the sample is displayed in degrees Centigrade.

n Current TG signal value

The TG signal is displayed in milligrams.

n Current hold temperature

During measurement, the hold temperature (final temperature) of the temperature

program in execution is displayed.
Except during measurement, the hold temperature of the first temperature program step
is displayed.

n TG±full scale value

The balance range (full scale value) which is now set is displayed. When autorange is
set, the characters "AUTO" are displayed.

6.3 Explanation of keys 6

The TGA main body has the keys shown in the following figure.

TEMP AUTO
START FUNC
PRG ZERO

STOP p q ENT

■ START (Start)

Used to start measurement.

By pressing this key after setting the temperature program, the furnace goes up
automatically to start measurement.
When the set temperature program has been executed, the measurement stops
automatically.

TGA-50/50H 27
 6 (APPENDIX)Detailed Explanation of keys

Upon completion of measurement, if POWER OFF is preset,the power supply of the

instrument is turned off when the temperature of the sample section falls below 500°C.

■ STOP (STOP)

Used to terminate measurement forcedly.

By pressing this key during measurement, the measurement terminates at that moment.
When measurement is forcedly terminated by the [STOP] key, the power
supply of the instrument is not turned off even if POWER OFF is preset.
If [STOP] is pressed concurrently with the [p] key or [q] key in setting temperature
programs, the indicated value changes 10 times as fast as with just the arrow key.
If this key is pressed while the furnace is going up or down, its movement can be
stopped.

TEMP
■ (Temperature program)
PRG

Used to set and display temperature program steps.

By pressing this key in the normal display mode, the first step of the program out of
up to 99 steps is displayed. In this condition, the temperature program can be set.
If this key is pressed in the normal display mode when a temperature program is executed
(the temperature rises), the program's current step is displayed.
If no key entry is executed for about 3 minutes while a temperature program step is
displayed, the display automatically returns to the normal display.
If this key is pressed when a temperature program step is displayed, the display returns
to the normal display at that moment.

AUTO
■ (Auto zero)
ZERO

Used to change the displayed values of the TG signal and differential signal to "0".
By pressing this key, the displayed value of the TG signal at that moment is changed to
"0 mg".
The recorder signal output is not affected by this operation. The signal through the
RS-232C becomes "0 mg" at that moment.
If no key entry is executed for about 3 minutes in the auto zero setting display mode,
the display automatically returns to the normal display.
If this key is pressed in the auto zero setting display mode, the display returns to the
normal display.

■ FUNC (Function)

Used to set the following items.

• TIME SCALE
• POWER KEEP/OFF
• PID
• FILE DELETE
• FILE SAVE

28 TGA-50/50H
 6.4 Temperature Program

• FILE LOAD
• CALIBRATION
• RANGE
If no key entry executed while the function setting screen is displayed, the display
automatically returns to the normal display.
If this key is pressed during function setting, the display returns to the normal display.
"6.6 TIME SCALE" to "6.13 RANGE（Weight signal range）"

■ p q (Arrow)

Used to change the value of the item where the cursor is positioned.
When the item where the cursor is positioned is a number, the [p] key increments it
and the [q] key decrements it.
When the item where the cursor is positioned is a character, this character changes in a
fixed sequence when an arrow key is pressed.
If these keys are pressed in the normal display mode, the furnace can be
moved up or down.
To stop the movement of the furnace, press the [STOP] key while the furnace is moving.

■ ENT (Enter)

Used to set or enter the value of the item where the cursor is positioned.
After changing the value of the item by the arrow keys, press this key. The value is
entered.

To change any setting, be sure to depress [ENT] key after altering the indication
of the item to be changed, otherwise the alteration cannot be input to change
the setting and the indication afterward returns.

6
6.4 Temperature Program
A temperature program can incorporate up to 99 steps, each of which consists of a
heating rate, hold temperature and hold time, as shown in the following figure.

A preset temperature program can be saved even if the power supply is turned off.
Unused temperature programs can be filed if desired.

TGA-50/50H 29
 6 (APPENDIX)Detailed Explanation of keys

Heating rate
A value ranging from -99.9 to 99.9 can be set (in units of °C/min or °C/hour).

The heating rate in practice is subject to limitation because of temperature zones

and types of coolant.

Hold temperature
• 0.0 to 1050.0 for the M type
• 0.0 to 1550.0 for the H type
can be set(in units of °C).

Hold time
A value ranging from 0 to 999 or infinity (...) can be set (in units of min or hour).

Temperature program setting

Press the [TEMP PRG] key.
The first step of the temperature program currently set is displayed.

Temperature program display

Movement of cursor
Each time the [ENT] key pressed, the cursor proceeds to the next item.

30 TGA-50/50H
 6.4 Temperature Program

If the [ENT] key is pressed when the cursor is at hold time position, the next step of the
temperature program is displayed.

Display of temperature program steps

When the cursor is positioned at a temperature program step number, press the [p] key
or [q ] key.
When the [q] key is pressed, the next temperature program step is displayed.
When the [p] key is pressed, the previous step is displayed.

Press the [p] key.

Press the [q] key.

Setting of heating rate, hold temperature and hold time

Position the cursor at the item to be set.

Set the desired value by using the [p] key or [q] key.

TGA-50/50H 31
 6 (APPENDIX)Detailed Explanation of keys

Entry by arrow keys

1 When the arrow key is momentarily pressed, the lowest-order digit of the
displayed number changes by one.

2 When the arrow key is continuously pressed, the digit changes every 0.5 second
or so.

3 When the key is released, the cursor returns to the lowest-order digit.
At the desired value to be set, press the [ENT] key.

To change the set value, be sure to press the [ENT] key finally.
Otherise, the displayed value can not be set and the original value
remains.

32 TGA-50/50H
 6.4 Temperature Program

Precautions for temperature programs

• If "0" is entered for the heating rate of a temperature program step, the subsequent
steps are initialized into "0".
For example, when "0" is set for the heating rate of temperature program
step 5, the subsequent steps including that of step 5 are deleted.
• The temperature program stops running before the step for which the heating rate is
set at "0".
For example, supposing the heating rate for step 3 is set at "0", measurement will end
at the end of the step 2 even if the 4th and 5th, etc., temperature program steps have
been set.
• A heating rate sign is automatically assigned by the difference between the hold
temperature of a step and the hold temperature of the next step.
For example, suppose that after the hold temperature of the first step is set at 300°C,
the second step is yet to be set (the hold temperature of the second step is 0). In this
case, if 20°C/min is set for the heating rate, "-20.0" is displayed.
In this condition, if 400°C is set for the hold temperature of the second
step, the heating rate turns to "20.0".

• If the temperature program directly set to the TGA main body and that set to the
personal computer (PC) are different from each other, the one to be executed is as
follows: 6
• When measurement starts after [START] key on the TGA main body is depressed,
Æthe directly set program is executed.

• When measurement starts after "START" button in "Acquisition: Status" window

is clicked on the PC screen,
Æthe PC set program is executed (and the directly set program is replaced with
the PC set one.
• While measurement is going on, it is possible to change the temperature program only
directly to the TGA main body.
When the currently executed program is to be changed, pay attention to the following
points.
• Heating rate: Do not change drastically.
• Target temperature: Once the program goes forward to a constant temperature
hold state, the status in quo never changes (the change is for the moment
ignored). The change only affects the subsequent runs of measurement. A void
changing a target temperature so as to cause a rate inversion from cooling to
heating as mentioned in Item 3.

TGA-50/50H 33
 6 (APPENDIX)Detailed Explanation of keys

• Constant temperature hold time: After the program goes on to the hold state,
the countdown of the hold time restarts from the newly set value as soon as the
setting is changed.
For example, if "10 [min]" is newly set for the hold time, the temperature is
thereafter kept constant for another 10 minutes.
• When measurement is over, the latest temperature program is written in the data file
of the TA-60WS for the run. So take care that the temperature program printed out
in the report can be different from that which was really executed as in the cases
described in Item 5. (Rewrite the program content according to the instruction manual
of the TA-60WS.) The temperature program table on the PC screen on the other hand,
is not replaced with the latest one upon the measurement end. Select "Upload All
Programs" item in the pull-down "Detector" menu to make the table content agree
with the latest program stored in the TGA main body.

6.5 AUTO ZERO

When operations for this function have been performed , the TG or differential signal
value display becomes "0 mg" or "0 mg/min". (However, the recorder output is not
affected.)
When the power supply is tumed off, the signal value returns to the original signal value
without undergoing auto zero, which comes from the detector.
The level meter indicates the actual level of the signal of the detector irrespective of
operations for auto zero.

Operations for auto zero

Press the [AUTOZERO] key.

Select a signal to which auto zero is to be applied, by using the [p] or [q] key.

Press the [ENT] key.

At this time, the TG signal or differential signal value becomes "0 mg" or "0 mg/min"
and the display returns to the normal display.

6.6 TIME SCALE

Item to set time units for the heating rate and hold time.
• For the heating rate, °C/min or °C/hour can be set.

• For the hold time, min or hour can be set.

34 TGA-50/50H
 6.6 TIME SCALE

Set time units can be saved even when the power supply is turned off. If a time unit is
changed when a temperature program is already set, the value remains as it is but its
unit is changed.
For example, if the unit of the hold time is changed from "min" to "hour" when "30
min" is set for the hold time, the set value becomes "30 hours".
The units of the set heating rate and hold time are displayed in the upper row of the
temperature program display screen.

Temperature program setting screen

Setting of time scale

Display the following menu by pressing the [FUNC] key and using the [p] or [q] key.

Press the [FUNC] key.

6
To change the unit of the heating rate, display the unit to be set using the[p] key or
[q] key when the cursor is positioned at the item "RATE". Then, press the [ENT] key.
The unit is set and the cursor proceeds to the hold temperature item.

To change the unit of the hold time, move the cursor to the item "TEMP" by using the
[ENT] key and display the unit to be set by using the [p] key or [q] key.

TGA-50/50H 35
 6 (APPENDIX)Detailed Explanation of keys

Then, press the [ENT] key. The unit is set and the display returns to the function display.

When the [FUNC] key is pressed finally, the display returns to the normal display. (If the
[FUNC] key is not press the display returns to the normal display in 3 minutes or so.)

6.7 POWER KEEP/OFF(power off)

Item to specify whether or not to turn off the power supply of the recorder upon
completion of measurement. If POWER OFF is set, the power supply of the recorder is
turned off and the LEDs on the panel and the liquid crystal indicator on the display unit
go out when the temperature of the sample falls below 500C after automatic completion
of measurement.
"POWER OFF" setting is convenient in case measurement ends in the absence of the
operator. When an analogue recorder is connected, unnecessary chart feed is avoided
with this setting.
For recovery from the automatic power off status, turn off the main switch (power switch
of the main unit) and turn it ON after a moment. The power supply may be recovered
automatically by a power failure. In this case, the power supply of the recorder is tumed
on but voltage is not applied to the heater.
Power off setting is released when the temperature program is aborted midway or the
power supply is turned off and on. To turn the power supply off automatically, set
POWER OFF on all such occasions.

Setting of POWER OFF

Display the following menu by pressing the [FUNC] key and the [p] or [q] key.

Press the [ENT] key.

To set POWER OFF by using the [▲] or [▼] key, display "OFF" and press the [ENT] key.
To reset POWER OFF, display "KEEP" and press the [ENT] key.

36 TGA-50/50H
 6.8 PID（PIO constants for temperature control)

After completion of setting, the screen is returned to the function menu display.

When the [FUNK] key is pressed finally, the display returns to the normal display.

6.8 PID（PIO constants for temperature control)

A special PID control system is adopted for temperature control. Each PID constant is set
to optimize the response of temperature control before shipment (default values: P = 10,
1= 10, D = 10). However, if optimum constants must be set again according to the
conditions of use or if the memory has been cleared, the PID function is available.
P： Applies a voltage to the heater in proportion to the difference between the preset
temperature and real temperature.
I ： Controls heater power to eliminate the difference between the preset temperature
and real temperature.
D： Controls the heater to equalize the slopes of the programmed temperature rise with
that of the real temperature rise.

Setting of PID
Display the PID setting menu by pressing the [FUNC]key and using the [▲] or [▼] key.

Press the [ENT] key.

Press the [ENT] key and move the cursor to the item to be changed. (At first, the cursor
is positioned at P.)

TGA-50/50H 37
 6 (APPENDIX)Detailed Explanation of keys

Change the displayed value into the desired value by using the [▲] or [▼] key and press
the [ENT] key.

The cursor moves to the next item automatically.

After changing a value ,be sure to press the [ENT] key, otherwise, the displayed value
can not be set.
If the [ENT] key is pressed when the cursor is positioned at D, the screen is returned to
the PID setting menu display. When the [FUNK] key is pressed finally, the display returns
to the normal display. (If no key entry is executed for 3 minutes or so, the display
automatically returns to the normal display.)

6.9 FILE DELETE（File deletion）

Operations to delete the measuring conditions stored in the memory. These operations
are performed to delete the measuring condition file of a specified number or all the
measuring condition files stored in the memory.

Operations for FILE DELETE

Display the file delete menu by pressing the [FUNC]key and using the [▲] or [▼] key.

Press the [ENT] key.

Display the number of the file to be deleted by using the [▲] or [▼] key.
• File numbers begin with "1".
• The existing file numbers are displayed in sequence by [▲] or [▼] key.
When file number "0" is selected, all files are deleted.

After the desired file number to be deleted is displayed, press the [ENT] key. A
confirmation display is made.

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 6.10 FILE SAVE（File saving）

After confirming that the displayed number is OK, press the [ENT] key. The file is deleted
and the screen is returned to the setting menu display.
If the number is not correct, press the [▲] or [▼] key. The file number to be deleted
can be changed.

Press the [FUNC] key last. The display returns to the normal display. (If no key entry is
executed for 3 minutes, the display automatically returns to the normal display.)

6.10 FILE SAVE（File saving）

Operations to file the measuring conditions currently used. The number of measuring
conditions that can be filed differs with the number of set temperature program steps:
for a one-step temperature program, 100 measuring conditions can be filed.

Operations for FILE SAVE

Display the file save menu by pressing the [FUNC] key and using the [▲] or [▼] key.

Press the [ENT] key.

Display the file number saving the measuring condition.

This number can not be changed.
After checking the number, press the [ENT] key.
The file is managed by only this number.
It will be convenient to separately record file numbers and their contents.
The measuring conditions currently used are saved as a file of the number selected.
The display returns to the setting menu display.

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 6 (APPENDIX)Detailed Explanation of keys

Press the [FUNC] key last. The display returns to the normal display. (If no key entry is
executed for 3 minutes, the display automatically returns to the normal display.)

6.11 FILE LOAD（(File call)

Operations to call a set of measuring Operations for FILE LOAD:conditions saved as a file.

Operations for FILE LOAD

Display the file load menu by pressing the [FUNC]key and using the [▲] or [▼] key.

Press the [ENT] key.

The smallest file number out of those that are currently saved is displayed.
Display the file number to be called by using the [▲] or [▼] key.

Press the [ENT] key.

The contents of the file are called and the display returns to the setting menu display.

Press the [FUNC] key last. The display returns to the normal display. (If no key entry is
executed for 3 minutes, the display automatically returns to the normal display.)

6.12 CALIBRATION（Calibration)
Item to set the gain or span of temperature and the gain of weight signal.
The temperature measured by the thermocouple is affected by the error of the
thermocouple itself and the atmosphere. These can be calibrated by key entries.
For temperature calibration, the following equation is used:
(Temperature) = (Measured temperature) x (Temperature gain) + (Temperature offset)
The temperature gain and temperature offset can be directly entered by keys. The
temperature gain and temperature offset can also be calculated and set automatically by

40 TGA-50/50H
 6.12 CALIBRATION（Calibration)

measuring the Curie point of nickel or if on and entering the literature value and
measured value. (2 points max.)
For weight signal calibration, the following equation is used:
(Weight signal) = (Measured value) x (Compensation gain)

Operations for CALlBRATION

Display the following menu by pressing the [FUNC]key and using the [▲] or [▼] key.

Press the [ENT] key.

The temperature gain and temperature offset currently set are displayed. To not change
gain setting, press the [ENT] key. To change the gain, display the desired value by using
the [▲] or [▼] key and press the [ENT] key.
The cursor proceeds to the offset item. Set the offset value in the same way. If the [ENT]
key is pressed when the cursors positioned the offset item, there appears the display for
entering the measured value and literature value. To not change the preset value， press
the [ENT] key repeatedly. When the [ENT] key repeatedly. When the [FUNC] key is
pressed,the display returns to the normal display.

6
First, display the literature value Curie point for the measured sample by using the [▲]
or [▼] key and press the [ENT] key to enter it into EXPECTED. The cursor proceeds to
MEASURED and the displayed value changes into the same value as the literature value.
At that time, set the measured value by using the [▲] or [▼] key and press the [ENT]
key. With this, the calibration for the first the first point is completed and the display
goes to the calibration point input display for the second point.

Perform the same setting as that for the first point. Lastly, position the cursor at the
measured temperature (MEASURED) position and press the [ENT] key. Then, the display
goes to the weight signal gain input display.

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 6 (APPENDIX)Detailed Explanation of keys

To change the gain value, set the desired gain value by using the [▲] or [▼] key and
press the [ENT] key. The display goes to the reference weight and measured value input
display.

Set the reference weight by operating the [▲] or [▼] key and press the [ENT] key.The
cursor proceeds to the right side and the displayed value changes into the input value.
Set the measured value by using the [▲] or [▼] key and press the [ENT] key.
The display returns to the first display for CALIBRATION.

What is noteworthy about the entry of a literature value and measured value
is that actual measurement must be made with the gain value and offset value
entered. If the gain value and offset value have been changed, return them to
the values for actual measurement and then reset them.

6.13 RANGE（Weight signal range）

Operations to select the full scale range of the weight signal.
There are 3 ranges available, i. e. ±20mg, ± 200mg and AUTO. With 20mg selected, the
range of ± 0.001mg to ±19.99mg can be measured. With 200mg selected, the range of
±0.01mg to ±199.9mg can be measured. When AUTO is selected, the same range as 20mg
is applied for measurement below ±20mg, or the same range as 200mg is automatically
applied for measurement over ±20mg.

Operations for RANGE

Display the following menu by pressing the [FUNC]key and using the [▲] or [▼] key.

When the above display appears, press the [ENT] key.

42 TGA-50/50H
 6.14 Error messages

Set the desired range by using the [▲] or [▼] key.

Press the [ENT] key. The range is set and the display returns to the initial function display.

Press the [FUNC] key last. The display returns to the normal display. (If no key entry is
executed for 3 minutes, the display automatically returns to the normal display.)

6.14 Error messages

n ROM 1 ERROR !

n ROM 2 ERROR !

The ROMs containing programs the checked when the power supply is turned on.
If any error is detected, this message is output. (After that, no key entry is accepted.)
Please contact the serviceman or business office.

n NO DETECTOR SIG !

The settings in the detector are read out when the power supply is turned on. If any
error is detected in the AMP setting in the detector, this error message is output.
Please contact the serviceman or business office.
6

n MECHANICAL FAULT !

This message is displayed when the furnace can not stop at a specified position after a
lapse of certain time while the furnace is moved up or down.
Check that the furnace is not caught by the cooling fan or others.

n HEATER FAILURE !

This message is displayed when the temperature of the detector does not go up even if
the heater is energized.
Check the heater and temperature sensor for broken wires.

n TEMP OUT OF RANGE !

This message is displayed when the temperature of the detector gets out of the setting
range.
Check the heating circuit and temperature sensor for abnormality.

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 6 (APPENDIX)Detailed Explanation of keys

n OVER CURRENT !

This message is displayed when a current over the rated value flows in the furnace
heater, and stops temperature control.
Do not perform an operation such as change of the PID values during temperature
control.

n POWER LIMIT !

This message is displayed when a current close to the rated value flows in the furnace
heater and provides control so as not to increase the current further. While this message
is displayed, the heating rate set in the temperature program is not followed.
When this message is displayed, the voltage of power supply is low or heating rate is
high. Set the voltage to high or heating rate to low.

n FURNACE IS TOO HOT !

This message is displayed if the furnace down key is pressed when the temperature of
the furnace is higher than 40°C.
Wait till the temperature of the furnace comes down.

n MEMORY FULL !

This message is displayed when the memory capacity insufficient to store another file.
Delete unnecessary files.

n FILE NOT EXIST !

This message is displayed when operations for FILE DELETE or FILE LOAD are performed
and the file is not found.

n SYSTEM CHANGED !

If RAM is initialized when power supply is turned on, or if switch S2 on the printed
circuit board PC-21D is changed, this message is displayed. Check to see if setting of
switch S2 is right. When RAM is initialized or switch 2 is changed, press the [ENT] key.

n POWER LIMIT OCCURED !

This message is displayed after the completion of the measurement surviving a POWER
LIMIT error.
The heating rate in the data obtained may not match one previously set.。

n NOT AVAILABLE !

This message is displayed when excessive correction is required upon temperature

calibration by the enter of a measured value and a literature value.
This message tends to appear, for example, when temperature calibration is performed
using two points too close to each other. As calibration reference points, use two points
having a difference of more than 500°C, or conduct one point calibration.
tumed off and the

44 TGA-50/50H