346-69810R

Mar. 2023

SIMULTANEOUS MEASUREMENTS OF
THERMOGRAVIMETRY AND DIFFERENTIAL
THERMAL ANALYSIS

DTG-60 DTG-60H

INSTRUCTION MANUAL

Read the instruction manual thoroughly before you use the

product.Keep this instruction manual for future reference.
 Introduction
Read this Instruction Manual thoroughly before using the
product.
Thank you for purchasing this product.
This manual describes the operation, 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 Instruction 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 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.
 Windows is a registered trademark of Microsoft Corporation in the United States and/or
other countries. Other company names, product names, service marks, and logos
mentioned in this manual are trademarks or registered trademarks of their respective
companies. The TM and ® symbols are omitted in this manual.

© 2000-2023 Shimadzu Corporation. All rights reserved.

Original version is approved in English.
Introduction

Indications Used in This Manual

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

Indication Meaning
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.

 Safety Instructions

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

 Product Applications
WARNING
Do NOT use the product for purposes other than those specified.
Using it for an unspecified purpose may result in an accident.

Safety regulations and standards

For notifications on installation and safety controls, follow the necessary
procedures in compliance with the laws and regulations applicable in the country
where the product is used.

 Installation Site
WARNING
Do NOT install the product in locations that are exposed to flammable or
explosive gases or liquids.
This product is not explosion-proof. Installing it in such an area may result in a fire
or explosion.

Do NOT place combustibles on top of the furnace.

This product exhausts hot air from the upper part of the furnace.If the hot air blows
directly on combustibles and burn them, they may cause burn and fire.

Install the instrument in a location that satisfies the following conditions.

Failing to do so may result in electric shock or fire.
• The room temperature is maintained between 5 and 40 °C, with minimal
temperature variation during a day.
• Air currents from heating or air conditioning equipment are not directed onto
theinstrument.
• Ensure that Instrument is not exposed to direct sunlight.
• There is no vibration.
• There is no condensation. (auto-cooling type:humidity is 80% or less)
• The location conforming to the installation environment (IEC)
(Installation category II, Pollution degree: 2, Altitude: Up to 2000 m, Indoor)

 Do NOT install the product in locations that are exposed to corrosive gases, gases containing
organic solvents/halogenated substances/siloxanes, oil mist, or large amounts of dirt or dust.
This may make it impossible to maintain the product's performance or shorten the life of the
product.
 Do NOT use the product in an environment where dew may condense on it.
This may prevent its normal operation.
 Install the product in locations where the power switch can be easily operated.
The power switch must be turned off in case of an emergency.
Introduction

 Installation
WARNING
 Do NOT place heavy objects on the power cord, and keep any hot items
away.
 Do NOT modify the power cord in any way. Do NOT bend it excessively or
pull on it.
The cord may be damaged, resulting in a fire, electric shock, or malfunction.
If the cord becomes damaged, contact your Shimadzu representative immediately.

 To ensure safe operation, contact your Shimadzu representative if product

installation, adjustment, or re-installation (after the product is moved) is
required.
Installing, adjusting, or re-installing the product by yourself may cause an injury
or equipment failure, or affect stable operation of the product.
 Take measures to prevent the instrument from falling in the event of an
earthquake or other disaster.
Strong vibrations may cause the instrument to fall over, resulting in an injury.
 The power supply voltage of the instrument is indicated on the label on the
rear side of the instrument. Connect the instrument only to a power supply
of the voltage indicated.
Otherwise, a fire or electric shock may result. Check that the power supply voltage
is stable and that its current capacity is sufficient to operate all the components of
the system. If not, the instrument will not operate at its rated performance.
 Ground the instrument.
Grounding is necessary to prevent electric shock in the event of an equipmen
failure or short circuit, and important for ensuring stable operation.
 Insert the power cord in the power outlet at an easily accessible position.
The power cord must be unplugged from the power outlet in case of an
emergency.

CAUTION
 Be aware of gaps around the instrument during installation.
If your fingers get caught, it may result in an injury.
 Ground the PC and the optional units with equal potential grounds.
Otherwise communications between units may be interrupted and equipment
failures may occur.

 Operation
WARNING
Do NOT measure explosive, ignitable, or flammable materials or inject them
into the instrument.
They may ignite and cause a fire.

Be careful about the heating furnace temperature. Avoid contact when it is

hot.
Contact may cause burn injury.
 Safety Instructions

 Inspection and Maintenance

WARNING
Never remove the main cover.
This may cause an injury or equipment failure.
The main cover does not need to be removed for routine maintenance, inspection,
and adjustment. Have your Shimadzu representative perform any repairs requiring
removal of the main cover.

 Unplug the power cord of the instrument before inspection, maintenance, or

parts replacement.
Otherwise, electric shock or short-circuit accidents may occur.
 When replacing a part, use the part described in the instruction manual.
If you use any other part, that part may be damaged, preventing normal use of the
instrument.

 Repair, Disassembly and Modification

CAUTION
Do NOT modify or disassemble the product without permission.
This may result in accidents due to electric shock or short circuits. It may also
result in an injury or equipment failure.

When repair is necessary, request your Shimadzu representative.

Failing to so may result in an ignition, electric shock, or injury.
Introduction

 In an Emergency
Emergency Shutdown Procedure
1 Press the STOP button on the front of the main unit.

2 Turn OFF the power switch on the main unit.

 During a Power Outage

Take the following measures in the event of a power outage.
1 Immediately turn OFF the gas supply.
2 Switch OFF the power to the main unit.
3 Open all windows and doors of the room to thoroughly ventilate it.
4 Wait until the temperature of all components of the main unit has fallen to the ambient temperature.
5 After confirming all related items in this section's Installation and Operation precautions, use the
standard startup procedure to start the instrument.
 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.

1
３

Warning
No. Description
Labels
(Part No. 037-72126-01)
1 HOT SURFACE
Avoid touching the furnace when at higher temperatures.
(Part No. 037-73006-11)
TOXIC EXHAUST
2
Take measures for draft when sample evolves toxic gas through pyrolysis
or reaction.
(Part No. 037-72006-00)
NEVER PINCHED
3
To avoid finger pinch, keep hands off the moving furnace/cellcover/cooling
jacket.
Introduction

Residual Risk Information

A residual risk indicates a risk that could not be reduced or eliminated in the process of design and
manufacture. Check the risk locations in "Residual Risk Map", and take the relevant protective
measures described in "List of Residual Risks".

 Residual Risk Map

The "Mechanical Location" and "No." indicated below are in accordance with those in "List of
Residual Risks". For details, see "List of Residual Risks".

Location A:Heating furnace upper part

No. 1

Location B:Heating furnace vicinity

No. 2

Location C:Heating furnace lower part

No. 3
 Residual Risk Information

 List of Residual Risks

The "No." and "Mechanical Location" indicated below are in accordance with those in "Residual Risk
Map". Be sure to check the actual "Mechanical Location" referring to "Residual Risk Map".
Furthermore, read through and understand the content in "Reference" to take appropriate protective
measures.
Opereation
Mechanical Protective Measure
No. Description - -
Location taken by machine user
Reference ■Operation
measurement
Operation
and
Category maintenance
Be careful about the heating
1 A furnace temperature. Qualified
Risk of burn injury Avoid contact when it is hot. Required person
received
Qualification/
training to
Education use the
instrument

Reference P.7
Measurement
Operation
 Ventilate well during generating a
Category gas
measurement.
2 B  When performing Qualified
Risk of poisoning measurement generating a person
Required
toxic gas, exhaust the gas. received
Qualification/
training to
Education use the
instrument

Reference P.5
Operation Heating
Category measurement
Keep hands away from the
3 C heating furnace while it is lifted Qualified
Risk of finger pinch person
up/down. Required
injury received
Qualification/
training to
Education use the
instrument
Introduction

Warranty
Shimadzu provides the following warranty for this product.
Please contact your Shimadzu representative for information about the period
1. Period:
of this warranty.
If a product/part failure occurs for reasons attributable to Shimadzu during the
2. Description:
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 1. In no event will Shimadzu be liable for any lost revenue, profit or data, or
of Liability: 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.

Failures caused by the following are excluded from the warranty, even if they
4. Exceptions:
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. Consumables and equivalent 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.
 Disposal Precautions

After-Sales Service and Availability of

Replacement Parts
After-Sales If any problem occurs with this product, perform an inspection and take
appropriate corrective action as described in "6.3 Troubleshooting" of
Service this manual.
If the problem persists, or the symptoms are not covered in the
troubleshooting section, contact your Shimadzu representative.

Replacement Replacement parts for this product will be available for a period of
seven (7) years after the product is discontinued. Thereafter, such
Parts Availability 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 the maintenance/inspection
section of this Instruction Manual.
 Periodic inspection/calibration should be requested to your Shimadzu representative.
 Replacement cycles described for periodic replacement parts are rough estimate.
Replacement may be required earlier than the described replacement cycles depending on
usage environment and frequency.

Disposal Precautions
This product contains battery/cadmium.
To dispose of it, ask an industrial waste disposer in compliance with the local laws and regulations.
Insulation material pieces must be disposed of in compliance with the respective national or local
government regulations.
Introduction
 Contents

Contents
1 Part List ........................................................................................................... 1

2 Part Names and Functions ............................................................................. 2

2.1 General View ....................................................................................................................2
2.2 Rear..................................................................................................................................3
2.3 Key/display section ...........................................................................................................4
3 Installation ....................................................................................................... 5
3.1 Instruction Requirements and Precautions .......................................................................5
3.2 Moving the Furnace Raise/Lower .....................................................................................6
3.3 Gas preparation ................................................................................................................7
3.4 Power supply ....................................................................................................................8
3.4.1 Connection with TA-60WS system ................................................................................... 9
3.5 Checking and Adjustment ...............................................................................................10
4 Operation for measurement ......................................................................... 12
4.1 Basic Operation ..............................................................................................................12
4.1.1 Starting up the devices ................................................................................................... 12
4.1.2 Sample preparation ........................................................................................................ 12
4.1.3 Setting sample pans ....................................................................................................... 12
4.1.4 Entering measurement conditions etc ............................................................................ 13
4.1.5 Starting and stopping measurement .............................................................................. 13
4.1.6 Measurement Stop ......................................................................................................... 14
4.1.7 Data analyses/correction ................................................................................................ 14
4.1.8 Making report .................................................................................................................. 15
4.1.9 Saving data file ............................................................................................................... 16
4.1.10 Modular Power Turn OFF ............................................................................................... 16
4.1.11 Precautions for handling ................................................................................................. 16
4.1.12 Supplement to gas handling ........................................................................................... 16
4.1.13 Caution in measurement ................................................................................................ 16
4.2 Preparation Related to Sample ......................................................................................17
4.2.1 Selection of sample pan ................................................................................................. 17
4.2.2 About sample .................................................................................................................. 19
4.2.3 About reference material ................................................................................................ 22
4.3 Gas substitution ..............................................................................................................22
5 Useful Functions ........................................................................................... 23
5.1 Measuring the Sample Weight with the DTG-60.............................................................23
5.2 Automatic Processing after Completion of Measurement ...............................................24
5.2.1 About template files ........................................................................................................ 24
5.2.2 How to set template file .................................................................................................. 24
5.2.3 Automatic Analysis ......................................................................................................... 25
5.2.4 Automatic Manipulation .................................................................................................. 25
5.2.5 Output ............................................................................................................................. 25
5.2.6 Canceling the template file ............................................................................................. 26
5.3 Configuring the Temperature During Standby.................................................................27
5.4 Auto Zero ........................................................................................................................27
5.5 Flow Controller ...............................................................................................................28
5.5.1 Setting Atmosphere Gas Condition ................................................................................ 28
5.5.2 Automatically Switching the Atmosphere Gas Condition Based on Temperature/Time . 28
5.5.3 Restoring the Atmosphere Gas Condition to the Original Condition After Completion of
Measurement ............................................................................................................................ 29
5.5.4 Displaying a Gas Name .................................................................................................. 30
5.6 Furnace Raise Prohibition Temperature/Fan Stop Temperature .....................................30

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Contents

5.7 Heater Control ................................................................................................................31

6 Maintenance and Troubleshooting .............................................................. 32
6.1 Maintaining the Performance ..........................................................................................32
6.1.1 Temperature calibration .................................................................................................. 33
6.1.2 Weight calibration ........................................................................................................... 35
6.1.3 Baseline adjustment ....................................................................................................... 36
6.1.4 Hold temperature adjustment ......................................................................................... 37
6.1.5 Cleaning run ................................................................................................................... 38
6.1.6 PID Parameters .............................................................................................................. 39
6.2 Troubleshooting ..............................................................................................................40
6.2.1 Error codes ..................................................................................................................... 40
6.2.2 Troubleshooting .............................................................................................................. 41
6.3 Maintenance ...................................................................................................................45
6.3.1 Consumables List ........................................................................................................... 45
7 Technical Data ............................................................................................... 46
7.1 Specifications .................................................................................................................46
7.2 Principle & Construction .................................................................................................47
7.2.1 Principle of measurement by DTG-60/60H .................................................................... 47
7.2.2 Standard materials used for calibration of DTA apparatuses ......................................... 49

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 DTG-60/DTG-60H

1 Part List
DTG-60/60H consists of the items listed below.
Check the contents with the list of items. If any items is found to have been missing or
damaged during transportation, please inform you forwarding agent and Shimadzu.
High Medium
No. Part name temperature temperatur
type e type
1 Main body DTG-60 for 120V AC
1 1
DTG-60H for 220/240V AC *1
The following parts are detached from the main body and packed together
with the standard accessories
Detector (PR) 2 2
Radiation cylinder (ceramic: for DTG-60H) 1 0
Radiation cylinder (ceramic: for DTG-60) 0 1
Furnace cover ASSY 1 1
Blower for cooling 1 1
Blower nozzle 1 1
A board for screw hiding 1 1
Balance unit 1 1
Standard accessories
2 Pt pans H2.5mm 0 3
Al crimp pans (50 pcs.) 0 1
Alumina pans H2.5mm 3 0
Platinum pan lid 2 0
3 Alpha-alumina 1 1
4 Tweezers ,K-23 No.3-120 1 1
5 Set of weights 1 1
6 Level 1 1
7 Silicon packing (50 pcs.) *2 1 1
8 Instruction Manual (this booklet ) 1 1
9 Service Manual (the other booklet) 1 1
*1 A step-down transformer or UPS is required (i.e., not included in this system).
*2 For reaction gas flow path. Used by field engineers during installation or failure.
1 2 3 4

5 6 7 8 9

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DTG-60/DTG-60H

2 Part Names and Functions

Name of each part is shown in the figure below.

2.1 General View

No. Name Description

1 Furnace cover
2 Detector
3 Tray for setting sample pans
4 Key/display section
Raise the furnace when placing a sample on the
detector.
While facing the unit directly, place the sample
container with the reference material on the left
side detector and the sample container on the right
side detector.
The sample can be placed on the hand rest before
and after measurements.
Consists of an LCD panel and operation keys.
2.3 Key/display section

- 2 -
 DTG-60/DTG-60H

2.2 Rear

No. Name Description

1 Power switch Turn the power on/off.
2 Fuse holder The fuse is set in the fuse holder.
3 Connector for TA-60WS Connects the DTG-60 to the TA-60WS interface.
cable
4 Connector for FC-60A cable Connects the DTG-60 to the FC-60A.
5 Gas supply ports Connectors for supplying the purge gas and dry
gas to the inside of the instrument.
6 Power cable Supplies all power to the instrument.

- 3 -
DTG-60/DTG-60H

2.3 Key/display section

No. Name Description

1 POWER Comes ON when the power is supplied to the main unit.
2 LCD Panel Usually displays the sample section temperature(in the unit of ℃).
When the [DISPLAY] key is depressed, displays the temperature →
TG signal(in the unit of mg) →DTA signal (in the unit of μV)
→temperature
3 Operation keys Perform the following operations.
This key is used to switch the LCD panel display
mode. Every time this key is pressed, the display
mode is switched in sequence: "Temperature" 
"Weight"  "Differential thermal analysis value" 
"Temperature". If any key on the DTG-60/60H is
not operated for at least 30 seconds after the LCD
is set to a display mode other than "Temperature",
the LCD will automatically return to the temperature
display mode.
Used to raise or lower the furnace cover. During
measurement, or when the sample temperature is
higher than the preset temperature, the furnace will
not be raised even if this key is pressed.
The weight or differential thermal analysis value
displayed on the LCD is reset to "0.00 (0)" or
"-0.00 (0)". The value displayed in the software is
set for 0.00 or -0.00 at the same time.
Normally not used. (Used by service person
for troubleshooting.)
 In emergency (upon detection of abnormality,
etc.), depress this key to cut the heater power
and terminate the measurement immediately.
Be careful not to depress this key by mistake
during measurement.
 If this key is pressed while the furnace is being
moved, the furnace will be stopped.

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 DTG-60/DTG-60H

3 Installation

3.1 Instruction Requirements and Precautions

1. For data acquisition, saving, analysis, report output, etc., the DTG-60/60H should be
connected to the Shimadzu Thermal Analysis System personal computer, printer, and
software, etc.
2. Prepare a power supply of 110 to 130V AC or 210 to 250V AC, High temperature type
(DTG-60H): 1500VA, Medium temperature type (DTG-60): 1300VA, single phase 50 or
60Hz. (A surge protector is recommended.)
3. To prevent an accident caused by electric shock or fire caused by electric leakage, be
sure to connect the ground cable to the ground terminal of the outlet of your power
supply.
4. To perform measurement in an inert gas (nitrogen, helium, or argon) atmosphere, install
the DTG-60/60H in a place where piping is provided, or use a compressed-gas cylinder.
For preparation of piping components and piping work, consult our authorized service
company. To perform measurement by supplying a reactive gas into the measuring
unit, be sure to purge the balance unit by supplying an inert gas. When a vacuum
pump is connected, the gas replacement in the measuring unit and balance unit can be
ensured.
5. To prevent gas leakage, be sure to mount a stopcock to an unused pipe connector.
6. Avoid installing in an environment exposed to direct sunlight or strong drafts, or where
there is vibration or excessive electrical noise, which may cause the microcomputer to
glitch.
7. Use the DTG-60/60H at room temperature between 5°C and 40°C, both inclusive, and
humidity of 80% maximum.
8. To suppress the influence of external vibration, install the DTG-60/60H on a solid
laboratory table or vibration-suppressing table. If the DTG-60/60H is installed in a
place where it is exposed to vibration caused by passage of automobiles, trains,
airplanes, people or closing/opening doors, highly-sensitive weight measurement may
not be performed. In general, the first floor or basement is more suitable for installation
of the DTG-60/60H, than upstairs. (Note that this may not be true depending on the
building structure.)
9. A fluctuation in room temperature may result in a drift in the DTG-60/60H's measurement
result. To obtain stable measurement data, do not install this instrument near an air
outlet of a cooler or heater. Be careful to minimize the fluctuation in room temperature.
10. If the DTG-60/60H is transported from the initial installation place, it will be beyond the
scope of warranty.
CAUTION
 Make at least 10cm space from adjacent equipment or wall on each
side.
Blocking the air inlet on the left side panel or the air outlet on the right
side panel may damage the instrument by decreasing the cooling
performance and overheating the internal components.

- 5 -
DTG-60/DTG-60H

474mm

650mm
367mm
Fig. 3.1 Dimensions

3.2 Stacking brackets

The use of commercially available stacking brackets is
recommended.
These brackets limit the possibility of the instrument
falling off the lab table during an earthquake or the
like. Various grades of stacking brackets are available.
Fasten the instrument firmly in place by attaching
stacking brackets to both the right and left sides two 1
locations (sheet metal part and plastic part) each, for a
total of four locations.For more details, contact your
Shimadzu representative.

3.3 Moving the Furnace Raise/Lower

Pressing the [OPEN/CLOSE] key can raise or lower the furnace.
Depending on the current status of the furnace, the [OPEN/CLOSE] key is activated as
follows:
Current status When [OPEN/CLOSE] key is pressed
When the furnace is at the upper position The furnace starts moving downward.
When the furnace is at the lower position The furnace starts moving upward.
While the furnace is being raised The upward movement is switched to the
downward movement.
While the furnace is being lowered The downward movement is switched to
the upward movement.
When the furnace is stopped between the The furnace starts moving upward.
upper and lower positions
Pressing the [STOP] key while the [OPEN/CLOSE] key is being activated stops the furnace.

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

While the furnace is open, [F.Open] is displayed. While the furnace is closed, [F.Close] is
displayed.

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 DTG-60/DTG-60H

3.4 Gas preparation

Fig. 3.2 Gas Flow Lines and Piping

The backside of the instrument has three gas ports for connecting gas piping.
(1) GAS1 (purge)
In this flow line, gas flows from the balance unit. Basically use GAS1 when performing
measurement with gas flowing into the sample section.
Flow rate reference values are listed below.
• When using air:
100 ml/min max.
• When replacing the atmosphere of the sample section with an inert gas
(nitrogen, helium, or argon):
Approx. 300 ml/min
(2) GAS2 (reaction)
In this flow line, gas flows directly into the sample section without going through the balance unit.
This line is used for special measurements, for example using air during measurement of carbon
black.
Example: Measurement of carbon black
At the start of measurement
GAS1 (purge): Nitrogen 200 ml/min
GAS2 (reaction): Nitrogen 100 ml/min
Switch to air during measurement
GAS1 (purge): Nitrogen 200 ml/min
GAS2 (reaction): Air 100 ml/min
(3) CLEANING
This line has a solenoid valve and is used for cleaning the furnace unit.
The flow rate is 200 to 300 ml/min for air.

The main unit does not include gas regulating valves and flow meters. To supply a gas,
provide the optional gas controller (FC-60A, etc.) additionally.
Supplying a large quantity of gas increases the baseline drift. It is recommended that the
gas flow rate should be within the range specified above.

- 7 -
DTG-60/DTG-60H

WARNING
 To prevent corrosion of the furnace or other parts, do not use a
corrosive gas (hydrogen chloride, etc.) as the reactive gas.
 Do NOT use flammable gases (such as hydrogen gas, gases
containing hydrogen, and acetylene).

 To prevent gas leakage, be sure to mount a stopcock to an unused pipe

connector.
 If the sample evolves a toxic gas during thermal analysis, a discharge
gas treatment device must be installed in the draft chamber, depending
on the density of the gas.

3.5 Power supply

Connect the power supply plug of the DTG-60/60H main body directly to a grounded outlet
with of 100/120 VAC, or connect it first to one of the socket-outlets of a step-down
transformer/UPS and second connect the power supply plug of the transformer/UPS to a
grounded-outlet) of 230 VAC. If grounded outlets are not available, use an adapter plug with
grounded contact, which should be securely grounded.
In the case of 100/120 VAC power supply…

100/120 VAC
DTG-60/60H
main body
socket-outlet

In the case of 230 VAC power supply…

100 VAC 230 VAC

DTG-60/60H
main body step-down
transformer/UPS
OUTPUT INPUT socket-outlet
Fig. 3.3 Power Supply Connection

WARNING
 Ground the instrument.
To avoid electric shock, supply electric power from a grounded outlet;
otherwise use a grounded adapter plug.

 Handle the power cord with care.

Observe the following precautions to avoid cord damage, fire, electric
shock,or instrument failure.
• Do not put heavy objects on the power cord.
• Keep hot items away from the power cord.
• Do not modify the power cord.
• Do not bend the power cord excessively or pull on it.
• Always pull the plug to unplug the instrument, NOT the power cord.
If the power cord is damaged, replace it immediately.

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 DTG-60/DTG-60H

3.5.1 Connection with TA-60WS system

In the TA-60WS system, a single personal computer can control up to four thermal analyzers
connected trough the interface. It allows connection of any of the 60 Series modules and
the 50 Series instruments*. Fig. 1.6 outlines the system configuration. For details, refer to
the software Instruction Manual.
* Some of the 50 series thermal analyzers cannot be connected with the TA-60WS system.
PC TA-60WS
Interface

DTG-60/60H

Thermal analyzer (up to 4 units)

Fig. 3.4 TA-60WS System Configuration

The following describes how to connect the DTG-60/60H with the TA-60WS interface.
Use the thermal analyzer connection cable (3m long) supplied with the TA-60WS interface to
provide a connection between the RS-232C connector at the top left corner of the rear panel
of the DTG-60/60H and one of the thermal analyzer connectors (CH1 through CH4; the
same type) on the rear panel of the TA-60WS interface.
For connecting another DTG-60/60H, use another thermal analyzer connector of the
TA-60WS interface. (Up to four units of the DTG-60/60H can be connected.)

RS-232C
1
POWER
2

3 Connector
4

To PC
TA-60WS interface
DTG-60/60H Rear Panel
Rear Panel

Fig. 3.5 Connection with TA-60WS interface

To control the DTG-60/60H, TA-60WS (Ver. 1.40 or greater) or LabSolutionsTA is required.

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DTG-60/DTG-60H
3.6 Checking and Adjustment
Check the following items after installation.
Step Operation
1 Turn ON the DTG-60/60H power switch.
The LCD panel on the key/display section
will momentarily display the character string
"Initial" and then start displaying the sample
section temperature. Wait for a moment
until the signal value is stabilized. (In this
status, the furnace must be at the lower
position.)
2 Depress the [DISPLAY] key. The LCD
panel display mode will switch to the TG
signal display mode.
3 Continuously, depress the [DISPLAY] key.
The LCD panel display mode will switch to
the DTA signal display mode.
4 Depress the [OPEN/CLOSE] key to raise
the furnace. On the right stage of the
detector plate, put a clean sample pan
somewhat warmer than the ambient
temperature.
5 On the left stage of the detector plate, put a
clean sample pan. Wait for a few minutes.
6 Depress the [ZERO] key after the TG signal
value becomes stable.
7 Depress the [ZERO] key after the DTA
signal value becomes stable.
8 Depress the [DISPLAY] key.
To perform the following checking procedures, the TA-60WS system is required. Start the
system and open the acquisition program. For the operation details, refer to the TA-60WS
Instruction Manual.
- 10 -
Check
 Check the sample section
temperature.
 Check that the temperature
indication is near the current
ambient temperature, with
fluctuation within about 0.5 C.
Check that the TG signal indication is
fixed or the significant digit (order of
0.01mg) changes sometimes.
Check that the DTA signal indication is
fixed or the significant digit (order of
0.1µV) changes sometimes.
At this time, check that the DTA signal
value increases to + side and after a
while gradually returns to the initial
value.
Make sure that the displayed weight
value changes to the saturated value.
Make sure that the displayed weight
value returns to the initial value.
Check that the TG signal indication is
set to 0.00 mg or -0.00 mg.
Check that the DTA signal indication is
set to 0.00 µV or -0.00µV
Check that the sample section
temperature display is resumed.
(After about three minutes from the
first pressing of the [DISPLAY] key for
switching to the other than temperature
display, the display mode automatically
switches back to the sample section
temperature display.)
 DTG-60/DTG-60H

9 Start measurement. Check that the sample section

Ex.） temperature begins to rise. Also
Temp. Rate Hold Temp. Hold Time check that the DTA signal value at first
15°C/min 300°C 0min changes drastically and then stabilizes
after about one minute.
And check that the TG signal value is
stability.

10 Terminate measurement. *1 Check that the measurement stopped.

* Depress the [STOP] key on the main unit or execute the measurement interruption procedures of the TA-60WS. In
the latter case, respond "NO" to data saving inquiry.

Now the checking procedures are complete. If any abnormality was found in any of the
above points, installation may be deficient or the instrument may be defective: after referring
to 6.3 troubleshooting, contact a Shimadzu service person.

 The sample temperature may not increase may not increase depending on the setup
of the computer.If the temperature does not increase, check the "Start data acquisition
** min. after measurement starts" item in the measuring parameters of the computer.
 During measurement (especially when heating up to higher temperature range), warm
air may flow out from the air outlet on the up side panel of the instrument. This
should not be regarded as abnormality. The air will not be so hot as to cause burns.

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DTG-60/DTG-60H

4 Operation for measurement

4.1 Basic Operation

4.1.1 Starting up the devices

1. Turn ON the power switches of the DTG-60, the TA-60WS interface, the personal
computer, the display unit, the printer, and any other peripheral devices.
2. When the Windows is activated, start the LabSolutions TA or TA-60WS software.
3. Start the acquisition program and select DTG-60.
Check the indicated values (the sample section temperature and the differential heat
flow) and graphs (temperature and heat flow transitions with time) to make sure that the
instrument is operating normally.

4.1.2 Sample preparation

1. Weight out the sample with a precision analytical balance.
At least 3 significant figures are necessary.
The element symbol is In. The purity should be preferably higher than 99.99%.
The readability of the balance must be 0.01 mg or 0.001 mg.
5.1
2. Put it standard aluminum sample pan.
3. Put an aluminum lid into the pan, and crimp it with an optional crimp press. (Shimadzu
SSCP-1 sample sealing crimp press for example.)
When a granular sample is prepared, it is better to crush it to a considerable extent
before crimping in order to keep the bottom face of the sample pan flat.
4. As for the reference material, use an empty aluminum sample pan of the same type,
covered with a lid and crimped in the same manner.
4.2

4.1.3 Setting sample pans

1. Depress the [OPEN/CLOSE] key to raise the furnace.

2. Put the pan containing the reference material on the left stage of the detector plate
(viewed from the front). And put the pan containing the sample on the right stage.
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 DTG-60/DTG-60H

3. Depress the [OPEN/CLOSE] key to descend the furnace, and wait until the TG signal
(weight value) is stabilized.

4.1.4 Entering measurement conditions etc

1. Select the [Measure] menu - [Add Sample] command in the acquisition program.
The "Setting Parameters" window opens.

2. Input parameters (Temperature program and File Information) to be measured.

3. Enter parameters, and select [OK] button.

4.1.5 Starting and stopping measurement

1. Make sure that the furnace is at the lower position, and then select the [Measure] menu
- [Start] command or select [Start] button on toolbar.
The following dialog box is displayed.

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DTG-60/DTG-60H

2. Input filename, Folder name and sample weight, and select the [Start] button.
 You can select a desired folder from a list of existing folders by selecting the
[Browse] button.
 When the [Read Weight] button is selected, the system reads the weight of the
sample mounted to the instrument, and displays the sample weight in the [Sample
Weight] field.
 When the [Take the initial TG signal for the sample mass] item is selected (this
check box is marked), the TG value sampled at the first point from the start of
measurement will be registered as the sample mass in the file information.This
function can be used for samples whose mass will be changed during preparations
for measurement, such as highly-volatile samples.
3. Measuring start, and the measured data is saved to the folder displayed in the [Folder]
edit box by the filename (ext. is tad) entered in the [File Name] edit box.

4.1.6 Measurement Stop

Normally, measurement is performed based on preset measuring conditions. After all
measurement conditions are satisfied, the measurement will automatically be completed.
This section describes how to stop measurement for any reason.

Selecting the [Measure] menu - [Stop] command in the acquisition program or selecting the
[Stop] button in the tool bar stops the processing of the now measurement.

4.1.7 Data analyses/correction

The TA-60WS system stores measurement data in the folder that the user specified at the
start of measurement by assigning the user-specified file name (with extension ".tad").
The completed measurement data can be displayed and analyzed according to the following
procedure:
1. Start the postrun program.
2. Select the [File] menu - [Open] command. The "Open" dialog box opens. Select the
desired file name.
3. After the data stored in the file will be loaded into the postrun program, the data can be
analyzed or corrected and then printed.
4. To save the data file, select the [File] menu - [Save] command. When changing the file
name, format, and/or disk location, use the [Save As] command.
Refer to software Instruction Manual for details.

Data analyses
Now perform the following procedures as required:
 To change the physical quantity or unit for the ordinate, or to change the line color or
type for the data curves:
the [View]-[Display Parameters] and subsequent procedures
 To change the scale factor for the abscissa or ordinate:
the [View]-[Scale Change] etc. and subsequent procedures
 To process or correct the data:
the [Manipulate]-[Smoothing] etc. and subsequent procedures
Then click the DSC curve. (A marker will appear at each end of the curve.)

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 DTG-60/DTG-60H

How to read the melting point (melting temperature)

Specify the point ("A" in Figure of an indium melting
peak") at which the DSC curve begins to depart from its
baseline, and the other point ("B" in the same figure) at
which the gradient of the ascending/descending part of
the peak becomes (quasi-) constant. Draw respective
tangent lines (AC' and BB') from the above two points.
The temperature value of the intersection point ("P" in the
figure) of the tangent lines is defined as the melting point
(melting temperature). The symbol "Tm" is generally used
for it.
Execute the [Analysis]-[Tangent] command, click Points A
and B, and click the [Analyze] button. The tangent lines
AC' and BB' will be displayed. To correct the gradient of
tangent line, drag at its end point (C' and B', espectively).
Clicking again the [Analyze] button displays the
temperature at Point P.

If the resulting value considerably differs from the literature value of the melting point of indium (out
of ±1ºC), perform temperature calibration followed by re-measurement/analysis.

How to obtain the heat of fusion (melting enthalpy)

Area (integration) between the interpolated baseline (line "AC" in Figure) during melting and
the subsequent transient state and the peak part of the DSC curve is theoretically proved to
be the heat of fusion (melting enthalpy), i.e., the total endothermic heat content (latent heat)
divided by the sample quantity, in the unit of, e.g., J/g. The symbol "DH" is generally used for
it.
Execute the [Analysis]-[Heat] command, click Points A add C, and click the [Analyze]
button. Line AC and the heat of fusion (melting enthalpy), as calculated from the peak area,
will be displayed. To change the unit, click the [Options] button and perform subsequent
procedures.]

If the resulting value considerably differs from the literature value of the heat of fusion of indium (out
of ±1.5J/g), perform heat flow calibration followed by re-measurement/analysis.

4.1.8 Making report

Select [View] and clear the checkbox on the [Sized with Window] command. Then click
[Format] and select the [Template] command to display the [Report Template] dialog box.
Select the file to refer to and click [OK]. The selected report format will be set.
 To relocate each displayed item or to change its character font etc.:
Click the displayed item to show its frame Drag the frame to relocate; double-click or
right-button-click the frame area to go to subsequent procedures for changing the font.
 To delete or add display item:
Click the displayed item to show its frame. Depress the [Delete] key (PC keyboard) to
delete; execute the [Insert]-[....] command to add a desired item with the either data
curve marked.
To confirm the print out image beforehand, execute the [File]-[Print Preview] command.
Execute the [File]-[Print] command to display the [Print] dialogue box. Check (and change as
required) the printing conditions and click the [OK] button. The report will be printed out.

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DTG-60/DTG-60H

4.1.9 Saving data file

Execute the [File]-[Save] command to save the data with the analysis results and its display
format information.
To change the file name or folder before saving, execute the [File]-[Save As] command
instead. If file name have been changed, the original name file will store the data with its
display format information, while the renamed file will store the data with the analysis results
and its display format information.

4.1.10 Modular Power Turn OFF

PC, TA-60WS interface and DTG-60 are turned off at the power switches.

4.1.11 Precautions for handling

CAUTION
Never turn off the DTG-60/60H with the furnace being in the lowered
position at its internal temperature of 500°C or more.
Otherwise, the temperature of the O-ring will increase, possibly
damaging it.

 Keep the O-ring located below the furnace clean. If the sample should be spilt
over the O-ring, remove it without giving any damage to it and then carefully
clean the O-ring groove. In addition, wipe off any foreign matter on the O-ring
and then fit the O-ring back to the groove.
 Any foreign matter like small dust between the sample holder and the sample
pan on the detector could deteriorate the thermal contact state, resulting in a
decrease in the sensitivity. Therefore, the utmost care must be taken for it.
Any foreign matter or scratch on the detector itself also deteriorates the stability
of measurement. If the detector becomes dirty during decomposition of a
sample, execute a cleaning run (see 6.1.3 "Cleaning run"), clean gently with a
cotton swab dipped in ethanol or acetone. Please note that applying strong
force may damage the balance. Never directly touch the detector with your
finger or anything else. If the foreign matter cannot be removed, it may be
necessary to replace the detector.
 Never apply strong force to the detector when cleaning it or when placing the
sample pan on the detector's sample holder. Otherwise, the detector will be
deformed and this can cause the drift base line.

4.1.12 Supplement to gas handling

To perform measurement in an inert gas atmosphere, keep supplying the inert gas for
approx. 10 minutes after lowering the furnace. In particular, for such a sample as is liable to
react with oxygen, previously evacuate the sample section with a vacuum pump before
sending the inert gas. This will make gas substitution more efficient.
4.3

4.1.13 Caution in measurement

1. The balance unit must be leveled. Using the level, which comes with the DTG-60/60H,
make sure that the balance always remains horizontal.
2. It takes some time before the DTG-60/60H has been stabilized after it is turned on.
When making an analysis at high sensitivity, it is recommended to allow the
DTG-60/60H to stand for one hour after turning it on or to keep the DTG-60/60H turned
on day and night.

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 DTG-60/DTG-60H

3. The detectors used for the DTA are of the same type on the reference substance (R)
side and the sample (S) side. However, if they are exchanged between the R and S
sides, the base line state will change. When analyses are repeated continuously, the
same pair of detectors should be used with their use limited to respective sides.
4. Since thermogravimetry is related to the gas phase, it is recommended to keep
supplying a gas around the sample to prevent a raise (or drop) in the partial pressure,
so that a constant atmosphere can be maintained during measurement to enhance the
data reproducibility and simplify the data analysis. Except for a case where a special
reaction is expected, make sure that air or inert gas is being supplied during
measurement.

4.2 Preparation Related to Sample

4.2.1 Selection of sample pan

When the target temperature is roughly 500°C or less, use the aluminum pan (with lid) which
is supplied as a standard accessory. For certain kinds of samples, it may be better to crimp
the pan.
If the target temperature exceeds 500°C, use the alumina pan (DTG-60H) or platinum pan
(DTG-60).
When measuring such a sample as reacts with any of the above materials for the sample
pan or triggers the catalytic action of platinum (for example, metal which forms alloy), use the
alumina pan. The platinum and aluminum pan cannot be crimped. To handle any liquid
sample, use the optional aluminum pan for sealing or the pressure tight aluminum pan.
Table 1 lists various types of sample pans. Use the suitable sample pan for your purpose of
analysis. For further details, contact us.

Keep in mind that detection sensitivity for heat and specific heat capacity varies depending
upon the kind of sample pans used.

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DTG-60/DTG-60H

Table 1 List of Sample Pans for DTG

Qty
Materia Dimension Capacity Upper limit
Part number Description in a Remarks
l s[mm] [µl] temperature
set
φ5.8×1.5
201-52943 Al crimp pans1) 34
(with lid) 600°C For general use
201-57268-90 Al macro-pans φ6×5 110
50 φ5.7×1.5 300℃
201-53090 Al Hermetic pans2) 34 Resistant up to 0.3
(with lid) max operating
Alumin MPa (lid with a
Al hermetic pans φ5.7×2.3 pressure0.3MP
um 222-13175-93 46 pinhole available)
(Deep type)2) (with lid) a5)
300℃
Al pressure-proof pans φ6×5 max operating Resistant up to 5
222-13073-91 3)
10 34
(with lid) pressure MPa
5)
5MPa
For general use,
201-51976 Pt pans φ5.8×2.5 60 expect for metal
fusion, sample
1300°C such as strong
Platinu basic substances,
201-53843 Pt macro pans 1 φ5.8×5 120
m alloy peroxides, iron
chlorides, and
halogen gas (Cl2,
201-56927 Pt pan lid φ5.7 - 1500°C Br2,…) evolving
samples.
Alumin 201-54321 Alumina pans φ5.8×2.5 50
1 1500°C For general use
a 222-13027-91 Alumina pan lid φ5.6 -
300℃
Resistant up to 0.3
4)
φ5.7×2.3 max operating
222-13175-94 Ag hermetic pans 50 46 MPa (lid with a
(with lid) pressure0.3MP
pinhole available)
a5)
For curing
reaction, samples
201-53102-84 Ni pans φ5.8×2 46 such as strong
Others basic substances
and peroxides
50 300°C
Suitable for
oxidation of
φ5.8×1.5
201-58294-90 Cu pans 34 polyethylene
(with lid)
(accompanied by
catalytic effect)
201-54439 Quartz pans 1 φ5.7×2.5 43 1,000°C
1) The SSCP-1 sample sealing crimp presss (S222-13130-91) and the crimp attachment (S222-13053-91) for crimping.
2) The SSCP-1 sample sealing crimp presss (S222-13130-91) and the sealing attachment (S222-12826-91) for sealing.
3) The SSCP-1 sample sealing crimp presss (S222-13130-91) and the pressure-proof pan attachment (S222-12915-91) for
sealing.
4) The SSCP-1 sample sealing crimp presss (S222-13130-91) and the Ag sealing attachment (S222-12826-92) for sealing.
5) For use upto upper limit temperature, as long as pressures do not exceed the max operating pressure.

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 DTG-60/DTG-60H

4.2.2 About sample

It is usual to measure a small amount of sample when it absorbs or generates a large
quantity of heat (i.e., produces a large peak), or a large amount of sample when it absorbs or
generates a small quantity of heat (i.e., produces a small peak).
To separate respective peaks of transitions/reactions occurring in succession, measure as
small an amount of sample as possible, which is spread as thinly and evenly as possible on
the bottom of the sample pan.
For calorimetry (heat measurement), measure an amount of sample that produces as large a
peak as possible, taking into account possible errors in measuring the peak area and the
noise level of the system, and also spread the sample as thinly and evenly as possible on
the bottom of the sample pan.
OK NG NG

Peak heights and shapes vary with heating rate. Heat the sample at 1 to 5 C/min when
peaks in concern occur very close to each other (resolution is the central issue) whereas at
10 to 30 C/min for calorimetry or when peaks are relatively small.
Keep the bottom surface of the sample pan as flat as possible to ensure good thermal
contact between sample and sample pan and between sample pan and detector plate.
Precautions are presented below for each of the various forms of sample.

Powder sample:
The particle size of a powder sample should be as uniform as possible to obtain
satisfactory measurement results. Sample of irregular particle size or containing extremely
large particle may produce shoulders in peaks.
OK NG

The powder diameter The powder diameter is

is even. uneven.

Granular sample:
A granular sample may be measured as it is, although it is usually sliced into thin pieces with
a knife. It may be cut into flaky pieces with a knife or ground into powder for measurement.
Keep in mind that polymer granules, e.g., plastic pellets, when suffering heat due to grinding,
result in a different DSC data from those of an original sample.

Film-like sample:
Film-like material is punched with the sample punch (The special attachments:
222-13586-91 or 222-13740-91) or cork borer or cut out by scissors to make a sample. If
the sample has various thickness, take a flake punched or cut out from one sheet with
such thickness as provides appropriate sample quantity rather than several thinner flakes
piled, in order to obtain a clear peak.

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DTG-60/DTG-60H

Fibrous sample:

Fibrous material is cut into small pieces to serve as sample. Fibrous samples are usually
deformed by heat, so they should be measured with the sample pan crimped together with
its lid. For crimping a sample pan, use the SSCP-1 sample sealing crimp press
(222-13130-91) and the crimp attachment.
About crimping (Aluminum crimp pan)
Crimping is to cover the sample-containing aluminum crimp pan with an aluminum lid, put
it in the sealer/crimper, and fold over the edge of the pan. Crimping improves thermal
contact, resulting in sharper peaks and stabile measurement results.

When the sample pan is crimped, the gas generated in the sample pans will not evaporate.
This may hinder a change in sample weight from being accurately measured. To measure
a change in sample weight, it is recommended that the sample pan should not be crimped.

Volatile sample:
For a liquid sample, a sample with high vapor pressure, or a solid sample containing such
substances, the latent heat of vaporization is lost during measurement. When the target
peak is small, therefore, the peak is hidden by the vaporization peak, or the baseline drifts.
In such cases, use a hermetic or pressure resistant sample pan or sealing pan to prevent
vaporization.

Others:
A paste sample is difficult to put in a sample pan. Do not try to put a large amount of
sample in the pan at once but apply it little by little on the bottom of the pan. Ensure that
the sample does not contain voids; because as the temperature rises, the voids would

- 20 -
 DTG-60/DTG-60H

expand, generating bubbles which procedure peaks as they are bursting resulting in noisy
data. If the sample sticks to the periphery of the sample pan or the pan bottom in contact
with the detector plate, wipe it off thoroughly. A trace amount of sample remaining in these
areas will soil the detector and cause noise.
Simultaneous measurements of any reaction in the solid phase and any decomposition
reaction. Use a needle to make about 20 holes on the Al lid for clamping use. In this
state, the decomposition pattern may slightly vary from that without closing the lid. (An Al
lid with pinholes is optionally available under Part No. 201-56586.)
As an application of the sealed pan, making holes of approximately 0.2mm dia. on the
sealed lid will allow the measurement of the boiling point. Such a sample pan for sealing
use with a pinhole lid provides almost atmospheric pressure inside, which prevents the
sample from overflowing.
Typical sample preparation processes have been briefly described. In short, it is important
to spread the sample over the sample pan bottom as thinly and evenly as possible to ensure
uniform temperature distribution in the sample and good thermal contact with the pan
bottom.
CAUTION
 Avoid measuring a sample whose thermal decomposition
products may stick to the furnace interior or detector. Also
avoid a sample which may possibly stick to the furnace interior
or detector when it boils.
Soiling of the furnace interior or detector will seriously deteriorate the
performance of the apparatus.
 Well clean the sample pans with organic solvent such as
acetone and dichloromethane.
 Samples Possibly Damage DTG-60/60H When Used Incorrectly.
Sample Possible Problem Remedy
Chlorine, When samples are heated  Flow the purge gas as much
Sulfurous gas, up to high as possible.
Volatile temperatures,.the detector  Reduce the sample size as
chloride such surface is damaged and its much as possible.
as Ammonia gloss is lost.  Use the minimum heat range.
Samples that When metals are liberated  Flow the purge gas as much
include due to high temperatures, as possible.
Antimony, the detector becomes  Reduce the sample size as
Selenium, brittle. much as possible.
Tellurium,  Do not heat up samples to
Phosphorus temperatures where metals
are liberated.
Silicic acid, When samples are heated  Do not heat up samples to
Silicate up to high temperatures, a temperatures where silicates
glass membrane is formed evaporate.
between the detector and
cell, and then they become
fixed together.
Metal lithium, When samples are heated  Sufficiently decrease the
Metallic in the air, almina melts. oxigeon concentration in the
sodium The alumina cell becomes furnace during measuement.
fixed to the detector.  Do not heat up samples to
temeperatures where metallic
vapor is generated.

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DTG-60/DTG-60H

4.2.3 About reference material

An empty sample pan or one containing powdered alumina (α - Al2O3) is generally used as a
reference. The rule of thumb is to use an amount of reference material is about twice the
weight of polymeric or organic material, or the same weight of inorganic material.
The pan containing the reference material must be of the same type as the corresponding
pan containing the sample. Specifically, crimp reference material pan when the sample pan
is crimped, and seal the former when the latter is sealed.

4.3 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, inert gas is filled up around the sample after with vacuum
pump connected balance case of this equipment, exhausting gradually for air inside furnace
and balance unit.
Repeating this operation three to five times enables the oxygen partial pressure to be
reduced in the atmosphere around the sample.

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

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 pinchcock, 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.
CAUTION
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.

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 DTG-60/DTG-60H

5 Useful Functions

5.1 Measuring the Sample Weight with the DTG-60

1. Depress the [OPEN/CLOSE] key to raise the furnace.

2. Put the pan containing the reference material on the left stage of the detector plate
(viewed from the front). And put the pan containing the sample on the right stage.

3. Depress the [OPEN/CLOSE] key to descend the furnace, and wait until the TG signal
(weight value) is stabilized.To supply an atmosphere gas, provide a gas flow meter.
(50 to 100 ml/min)
4. After the TG signal is stabilized, press the [DISPLAY] key. When the LCD panel
displays a weight value, press the [AUTOZERO] key. Then, the displayed weight value
becomes "0.00" (in the unit of "mg").
5. Press the [OPEN/CLOSE] key to raise the furnace, and take out the right sample pan.
Put a proper quantity of sample into the pan, and re-mount it onto the DTA detector.
6. Press the [OPEN/CLOSE] key to lower the furnace. The weight value displayed after
the TG signal is stabilized indicates the sample weight.

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DTG-60/DTG-60H

5.2 Automatic Processing after Completion of

Measurement

5.2.1 About template files

The template file is essentially a format file which will manipulate, analyze and/or output the
data file in a standard format.
To create template file for repeated sample analysis on similar samples, open typical sample
file, manipulate and/or analyze data, and save as a template file. Then apply the template file
to all subsequent samples with similar properties.

5.2.2 How to set template file

Create a template file to acquire a report format and analyzing/manipulating conditions.
If a report format and analyzing/manipulating conditions need not be obtained after
completion of measurement, the template file setting procedure is not necessary.
1. Execute [Measure]-[Set Template].

2. Specify a template file name to be used, and check repeat item.

3. If any analyzing/manipulating condition set in a template file becomes unnecessary or

another items must be added to the template file, you can edit the template file in the
Postrun Program.
4. Select the [OK] button.

When entering a file name, be sure to specify the full pathname starting from the drive
name.
Ex.) C: tadata template.tad
When the [Browse] button is pressed, the "Open" dialog box will be opened. You can
select a file name while browsing files.

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 DTG-60/DTG-60H

5.2.3 Automatic Analysis

If you select a Template file, an acquired data file will be analyzed according to the protocols
set in the template file. You can perform the following analyses with this function.
 Time/Temp Analysis  Signal Difference Analysis  Area Analysis
 Tangent Analysis  DSC Peak Analysis  Weight Loss (Auto) Analysis
 Peak Analysis  Glass Transition Analysis  Weight Loss Analysis
 Peak Height Analysis  Heat Analysis  Weight Loss Ratio->Temp/Time Analysis

How to perform an automatic analysis:

1. Execute [Measure]-[Set Template].
2. Specify a template file name to be used, and check [Perform Analysis].
3. Select the [OK] button.
4. After measurement, the automatic analysis will be performed according to template file.

To analyze a file that has already been measured, analysis in Postrun Program manually.

5.2.4 Automatic Manipulation

If you select a Template file, an acquired data file will be manipulated according to the
protocols set in the template file. You can perform following data manipulations with this
function.
 Smoothing
 Heat Correction
 Derivative
 Temperature Correction

How to perform an automatic manipulation:

1. Execute [Measure]-[Set Template].
2. Specify a template file name to be used, and check [Perform Manipulation].
3. Select the [OK] button.
4. After measurement, automatic manipulation will be performed according to template file.

To manipulate a file that has already been measured, manipulate in Postrun Program
manually.

5.2.5 Output
The file can be printed automatically after the measurement is completed.

How to output data:

1. Execute [Measure]-[Output].

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DTG-60/DTG-60H

2. Check [Print out]. Select the [OK] button.

3. After measurement, the file will print automatically.

5.2.6 Canceling the template file

Cancel the template file specifying the measurement data report format.
1. Select the [Measure] menu - [Set Template] command The "Set Template" dialog box
opens.
2. Select the [Clear Template] button, or delete all characters displayed in the [Reference
file name] edit box.
3. Select the [OK] button.
4. A message box appears, asking you if you wish to use the default template. Then,
select [Yes].
After this step is completed, data files will be saved in the format that displays a graph
at the center of paper.

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 DTG-60/DTG-60H

5.3 Configuring the Temperature During Standby

When the temperature is programmed, the module holds at the specified temperature.
Once the sample set temperature is set around the measurement start temperature for
repeated measurements at the room temperature and higher temperatures, the system holds
the set temperature at the preset temperature after the start of measurement. This function
can simplify the subsequent measurement procedure. When the sample holds temperature
is programmed, the module holds at the specified temperature.
This function can be terminated by pressing the [Stop] button.

1. Click [Sample Hold Temperature] on the [Measure] menu of the acquisition program.
The window for configuring the sample hold temperature is displayed.
2. Click [OK].
The sample temperature heats or cools to the programmed temperature and the module
waits at that temperature.
3. If "Continuous Hold Temperature" has been selected in the sample setup temperature
setting dialog box, the module will hold at the specified temperature after completion of
measurement.

5.4 Auto Zero

The latest signal value displayed on the acquisition program on the monitor screen can be
reset to "0.0".

1. To reset the TG signal value to "0", select the [Detector] menu - [AutoZero (TGA)]
command. To reset the DTA signal value to "0", select the [Detector] menu - [AutoZero
(DTA)] command. Then, select the [AutoZero] command below.

[AutoZero] : This command sets the current signal value to zero.

[ClearZero] : This command cancels the [Auto Zero] command and returns the
signal value to the original.

To restore the signal value to the original value, perform the following procedure.

1. Select the [Detector] menu - [AutoZero] command, and then select the [ClearZero]
command below.

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DTG-60/DTG-60H

5.5 Flow Controller

This command can be functioning when the optional accessories FC-60A supplies 2 line
atmospheric gas to the instrument.

5.5.1 Setting Atmosphere Gas Condition

The atmosphere gas can be supplied or cut off, regardless of whether measurement is being
executed or not.
The check mark appearing in front of the command shows the current setting.

1. In the acquisition program, select the [Detector] menu - [Flow Controller 1] command or
[Flow Controller 2] command (either flow controller connected to the atmosphere gas).
Then, select either the [Open] or [Close] command below.

[Open] : This command flows gas connecting the purge 1 (or purge 2) of FC-60A.
[Close] : This command stop the gas.

2. When the [Open] command is selected, the solenoid valve in the FC-60A will be opened
to supply gas connecting the purge 1 (or purge 2). When the [Close] command is
selected, the solenoid valve in the FC-60A will be closed.

5.5.2 Automatically Switching the Atmosphere Gas

Condition Based on Temperature/Time
1. Select the [Detector] menu - [Flow Controller 1] command, and then select either the
[Open] or [Close] command below to open or close the gas connected to purge 1 in the
FC-60A.
2. Select the [Detector] menu - [Flow Controller 2] command, and then select either the
[Open] or [Close] command below to open or close the gas connected to purge 2 in the
FC-60A.
3. Select the [Measure] menu - [Measuring Parameters] command or select button on
toolbar. The "Setting Parameters" dialog box opens.Mark the [FC Control] check box
on the "Temperature Program" property page by using the mouse. The [Gas] column
(parts of surround by circle) will be changed white color, and it becomes to set user's
input.

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 DTG-60/DTG-60H

Description on the program of front page

In the initial condition, Gas 1 is supplied and Gas 2 is not supplied.

When the program is switched from the first step to the second step, Gas 1 is
stopped, and Gas 2 is supplied.
4. Mark the check box corresponding to the gas number to be switched with the mouse,
and then select the [OK] button.
After the gas switching conditions are set, the DTG-60/60H will open or close the
corresponding gas supply port according to the normal temperature program. Each item of
the temperature program indicates the following condition:
Gas 1, 2 : Indicates the ON/OFF condition of the gas connected to purge 1 or
purge 2 in the FC-60A.
Hold Temp. : Indicates the temperature at which the gas switching operation is
executed.
Hold Time : Indicates the hold time required to execute the gas switching
operation after the sample temperature reaches the preset switching
temperature.

5.5.3 Restoring the Atmosphere Gas Condition to the

Original Condition After Completion of Measurement
When the atmosphere gas is automatically switched based on the FC temperature control
program, the gas condition specified in the final step of the temperature program will be
retained after completion of the measurement.
To restore the gas condition to the original condition after completion of measurement,
perform the following procedure.
1. Select the [Detector] menu - [Detector Properties] command. The "Detector
Properties" dialog box opens.
2. Select the [Flow Control] tab by mouse. The "Flow Control" Property displays.
3. Select the [Return the initial gas after measuring] check box.

4. Select [OK] button. The updated condition will be activated after the next measurement
is started.

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DTG-60/DTG-60H

5.5.4 Displaying a Gas Name

When the gas switching conditions have been set, the temperature program displayed in the
report format is as follows:
Temp. Rate Hold Temp. Hold Time Gas
10 300 10 1
A specified gas name can be displayed in the [Gas 1] column.
1. Select the [Detector] menu - [Detector Properties] command. The "Detector
Properties" dialog box opens.
2. Select the [Flow Control] tab by mouse. The "Flow Control" Property displays.

Gas 1 : Set the gas name of the purge 1 of the FC-60A.

Gas 2 : Set the gas name of the purge 2 of the FC-60A.
When input "Air" on the Gas 1.
Temp. Rate Hold Temp. Hold Time Gas
10 300 10 Air

3. Select the [OK] button.

5.6 Furnace Raise Prohibition Temperature/Fan

Stop Temperature
The DTG-60/60H can control the furnace raising operation and stop the fan based on
temperature.
1. Select the [Detector] menu - [Detector Properties] command of the acquisition program.
The "Detector Properties" dialog box opens.
2. Select the [DTG-60] tab by mouse. The "DTG-60" property displays.

3. Normally, the furnace raise prohibition temperature is set to "50.0C ". However, this
setting can be changed. When the furnace temperature falls below the preset
temperature, the furnace can be freely elevated.

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 DTG-60/DTG-60H

4. Normally, the cooling fan control is set to "Control" "40.0C". However, this setting can
be changed as follows:
[ON] : The cooling fan is running.
[OFF] : The cooling fan is OFF.
[Control] : The fan stop temperature can be set to a desired temperature. When
the furnace temperature falls below the preset temperature, the cooling
fan stops.

5. After changing the setting, select the [OK] button.

5.7 Heater Control

The DTG-60/60H can determine whether the furnace temperature or the sample temperature
is used to control the temperature in the furnace.
1. Select the [Detector] menu - [Detector Properties] command of the acquisition program.
The "Detector Properties" dialog box opens.
2. Select the [DTG-60] tab by mouse. The "DTG-60" property displays.

3. To use the furnace temperature, select the [Use furnace temperature] item; or to use the
sample temperature, select the [Use sample temperature] item, by using mouse.
Then, select the [OK] button.

When machine controls by the sample temperature, temperature curve can't sometimes
carry out of temperature program by endothermic/ exothermic point.

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DTG-60/DTG-60H

6 Maintenance and Troubleshooting

6.1 Maintaining the Performance

For confirming quantitatively the instrument's performance, measure the melting temperature
and the heat of fusion (melting enthalpy) of a standard material before taking measurements
on samples: compare measured values with literature values (or validated values shown in a
document attached to the standard material). Here is an example criterion in the case of
pure indium, the most conveniently used standard material:
Melting temperature : (156.63 ±1.0) °C
Heat of fusion : ( 28.5 ±1.5) J/g
If the melting temperature or the heat of fusion as actually measured by the instrument is not
within the above range, calibrate the instrument. Note, however, that the users may use their
own criterion of accuracy allowances.
Measure the melting temperature and the heat of fusion of a standard material
according to the procedures described in "How to read the melting point
(melting temperature)", and compare the measured values with the respective
literature values.

Maintenance and Inspection Task List

The maintenance and inspection timings listed in this table are presented only a guidelines.
These timings do not represent a guaranteed period of service.
These timings differ depending on the conditions of use.
Inspection/ 1 1
other Remarks See
Maintenance Item week month
Temperature calibration ✓ ✓ - 6.1.1
Weight calibration ✓ ✓ - 6.1.2
Baseline adjustment ✓ ✓ - 6.1.3
Hold temperature adjustment ✓ ✓ - 6.1.4
Cleaning run - - ✓ When organic matter 6.1.5
adheres to the detector
If there is, however, a corporate standard, e.g., one established as the GLP, conform to it.
After every cleaning run or detector replacement, necessitated when the furnace or the
detector is soiled, be sure to perform this quantitative evaluation of the accuracy.
(After detector replacement, however, a Shimadzu service person will perform this
procedure.)
To ensure that the instrument is always in its best condition, it is recommendable that the
user signs a maintenance agreement with a Shimadzu service company that stipulates
periodic (usually annual) inspection.

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 DTG-60/DTG-60H

6.1.1 Temperature calibration

The temperature calibration is performed based on the following equation:
(Expected temperature) = (Measured temperature) + T
The correction term ΔT in the above equation is temperature-dependent, and can be
approximated by the following linear equation:
ΔT(Tm) = A＋B×Tm
Where, T(Tm) is the correction value at the temperature Tm, while A and B are respectively
the zero-order and primary-order calibration coefficients. Even though it is also possible to
directly specify the values A and B, we recommend a method in witch these values are
replaced with automatically calculated ones by inputting the actually measured melting
temperature of the standard material and its literature (or supplier-validating) value.
1. Start the LabSolutions TA or TA-60WS software.
2. When you click the mouse on the module name (ex. DTG-60) to be calibrated , the
acquisition program is displayed at the top, and the monitor window of the selected
module is displayed.
3. Execute the [Detector] menu - [Temperature Calibration] command to display the
"Temperature Calibration" window.

4. Click the [Calculate] button. The "Temperature Calibration Coefficient" window is

displayed.

5. Enter the name of the standard material used in the [Standard Sample Name] column,
the literature melting temperature in the [Expected] column, and the measured melting
temperature in the [Measured] column, respectively.
Some names of often-used standard materials can be selected from the list. For these
materials, the literature value is automatically entered in the table.
6. Finally click the [OK] button to display the newly calculated values of A and B.

If only one standard material was used for calibration, only the value of A is changed.
If two standard materials were used, the values of A and B are given as solutions of a linear
equation.
If three or more standard materials were used, the values of A and B are determined as
coefficients of a primary regression line in the least square approximation.
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DTG-60/DTG-60H

If the material or shape of the sample pan or the type of the atmospheric gas is different
from those used for calibration, the measured melting temperature may fluctuate. Such
fluctuation must be corrected later on in the data analysis stage.

7. To update the calibration coefficients (i.e., to send the newly calculated values from the
PC to the DTG-60/60H), click the [Download] button, read the message in the message
box, and clicks the [Yes] button. After confirming the calibration data, which is
hereupon renewed, click the [Exit] button to terminate the procedure.

If there is no change in the calibration coefficient, a message appears asking you if you
wish to change only the calibration date before sending the calibration coefficient. If you
wish to change the calibration date only, select [Yes]. If you wish not to add any change,
select [No].
Note that the updated calibration date cannot be restored.

About substance for temperature calibration

The temperature measurement involves an error occurring from the temperature-sensing
element itself in addition to errors resulting from various external factors. Therefore, in
order to obtain the accurate temperature, the temperature must be calibrated under the
prevailing conditions. The simplest way for the temperature calibration is to measure the
melting point of pure metal. The standard calibrating material should be tested under the
same conditions used for the sample. Obtain the fusion starting point from the acquired
fusion peak and then compare it with the cited melting point. Thus, the temperature
calibration for the DTG-60/60H can be carried out.
The melting points of typical pure metals of 99.9% minimum are listed below:

Melting point (°C)

Indium 156.5985
Tin 231.928
Lead 327.50
Zinc 419.527
Aluminum 660.323
Silver 961.78
Gold 1064.18
* The cited values are based on the "Rika Nenpyo, 2016 Edition."

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 DTG-60/DTG-60H

6.1.2 Weight calibration

Set a weight calibration factor for module.
The temperature calibration is performed in the module, based on the following formula:
Wc   A  B  Tm   Wm
Wc : Weight after calibration (Weight output from the module)
Wm : Weight before calibration (Weight detected by the module)
Tm : Temperature during calibration (Temperature detected by the
module)
A : Weight calibration factor (Constant term)
B : Weight calibration factor (Linear term)

1. Start the LabSolutions TA or TA-60WS software.

2. When you click the mouse on the module name (ex. DTG-60) to be calibrated, the
acquisition program is displayed at the top, and the monitor window of the selected
module is displayed.
3. Execute the [Detector] menu - [Weight Calibration] command to display the "Weight
Calibration" window.

4. Click the [Calculate] button. The "Weight Calibration Coefficient" window is displayed.

5. Enter the reference value (document value), measured value and temperature during
measurement.

The calibration coefficient is calculated based on the ratio of reference value to measured
value. Even if the unit of each input line is different, it does not cause a problem.
For a calculation aren't problem if you input standard value and a measurement value of on
line one with mg, input a standard value and a measurement value of on line 2 with %, for
example. Please do for a same unit for a standard value and a measurement value of the
same line, however.
To obtain only "Coefficient A", fill in one line only.
6. Click the [OK] button. A new calibration coefficient will be calculated based on the
current calibration coefficient and the input values in the table. The newly obtained
coefficient will be displayed in the "Weight Calibration" dialog box.
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DTG-60/DTG-60H

7. To update the calibration coefficients (i.e., to send the newly calculated values from the
PC to the DTG-60/60H), click the [Download] button, read the message in the message
box, and clicks the [Yes] button. After confirming the calibration data, which is
hereupon renewed, click the [Exit] button to terminate the procedure.

If there is no change in the calibration coefficient, a message appears asking you if you
wish to change only the calibration date before sending the calibration coefficient. If you
wish to change the calibration date only, select [Yes]. If you wish not to add any change,
select [No].
Note that the updated calibration date cannot be restored.

6.1.3 Baseline adjustment

When exchanging a detector, by each characteristic dispersion on the side of sample and a
standard material, may cause the baseline to deviate with respect to the time axis or to
become non-linear during temperature heating or cooling (called baseline drift). In this
case, the DTG-60/60H is provided with the baseline adjustment function to correct a baseline
drift.
The following describes the procedures for baseline adjustment.

1. Start the LabSolutions TA or TA-60WS software.

2. When you click the mouse on the module name (ex. DTG-60) to be calibrated , the
acquisition program is displayed at the top, and the monitor window of the selected
module is displayed.
3. To adjust the TG signal baseline, select the [Detector] menu - [Baseline Adjust (TGA)]
command. To adjust the DTA signal baseline, select the [Detector] menu - [Baseline
Adjust (DTA)] command. Then, the "Baseline Adjust" window is displayed.

TGA DTA
4. By specifying the K-value in the following expression, correct the linear inclination of the
baseline (with respect to temperature):

K (mg or μV)
Bc = Bm + ×Tm
100(℃)

Bc : DTA (µV) or TGA (mg) signal after adjustment

Bm : DTA (µV) or TGA (mg) signal before adjustment
Tm : Temperature(°C)
K : Baseline adjustment factor (µV or mg)
To obtain the K-value, determine the amount of heat flow deflection (in the unit of mg or
µV) per 100 C from the original baseline. If the drift indicates a weight increase (TG)
or exothermic reaction (DTA), K is a negative value. If the drift indicates a weight
reduction (TGA) or endothermic reaction (DTA), K is a positive value. If the drift is
non-linear, the K-value will vary with temperature ranges. In this case, it would be

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 DTG-60/DTG-60H

advisable to select for K-value determination at 100 C including (or included in) the
target temperature range, in which a phenomenon of interest can be observed as, e.g.,
a peak.
5. After entering the K-value, click the [Download] button, read the message in the
message box, and clicks the [Yes] button. The K-value in the "Coefficient" column as
well as the adjustment date in the "Date" column will be updated. (The new K-value is
sent from the PC to the DTG-60/60H.)
6. Finally click the [Exit] button to terminate the procedure.
Conversely, the TA-60WS software and LabSolutionsTA provides various menus that can be
used for correcting a baseline after measurement. For details, refer to the software
Instruction Manual.

Baseline correction is possible also in the data analysis stage that follows the measurement
stage. However, we recommend to enforce a base line regulation of the case that base
line drift is remarkable equipment.

6.1.4 Hold temperature adjustment

When the equipment is controlled based on the furnace temperature (see 4.5), the sample
temperature may be held at a temperature slightly deviated from the target temperature
specified with the temperature program, depending on the temperature distribution in the
furnace.
Therefore, the actual sample hold temperature can become close to the preset target
temperature, if the deviated temperature is added to, or subtracted from the target
temperature (hold temperature) beforehand.

Example: To hold the furnace temperature 3.0 C lower than the target temperature, set the
hold temperature coefficient to "3.0 C". When a hold temperature has already been
set, add "3.0 C" to the programmed temperature.)

The following describes the procedures for offset temperate.

1. Start the LabSolutions TA or TA-60WS software.
2. When you click the mouse on the module name (ex. DTG-60) to be calibrated, the
acquisition program is displayed at the top, and the monitor window of the selected
module is displayed.
3. Execute the [Detector] menu - [Hold temperature adjust] command to display the "Hold
temperature adjust" window.

4. Enter the offset value between the actual sample temperature and the target
temperature specified on the temperature program. When the sample temperature is
lower than the preset temperature, enter a positive value. When the sample
temperature is higher than the preset temperature, enter a negative value.
5. Finally click the [OK] button to terminate the procedure.

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DTG-60/DTG-60H

6.1.5 Cleaning run

Substances generated from the measured sample may adhere to the furnace or detector. If
measurement is conducted in this state, the system may not provide the intended
performance. Therefore, when the system is to be used (1) for the first time after it is
purchased or (2) after a long period of rest perform a cleaning run. Through the cleaning
run, the substances adhering to the sample surface are decomposed and vaporized, so that
the clean surface can be obtained.
The following describes the cleaning run procedure.

1. Start the LabSolutions TA or TA-60WS software.

2. When you click the mouse on the module name (ex. DTG-60) to be calibrated , the
acquisition program is displayed at the top, and the monitor window of the selected
module is displayed.
3. Execute the [Detector] menu - [Cleaning Run] command to display the "Cleaning Run"
window.

With the above settings, the cleaning gas is supplied to the sample section immediately
as the cleaning run starts; the temperature is rapidly increased up to 600 C and it is
kept constant at 600 C for 5 minutes. To modify the cleaning conditions, change the
value or setting in each item box as required.
4. Finally click the [Start] button to start the cleaning run.

For effective cleaning, we recommend in most cases to supply the dry air (200 ~ 300ml/min)
as the cleaning gas. (Refer to 2.1 Gas preparation) when a cleaning run without gas
supply or with a purge gas supplied is to be conducted, set as follows:

Cleaning gas: No use

No data are acquired during a cleaning run.

 Conduct a cleaning run when the system has been out of service for about two weeks,
although the surface state depends on the operating conditions for the last
measurement and the storage conditions.
 Before conducting a cleaning run, make sure that no sample pans are left on the
detector plate. (Click both the sample and reference material sites.)

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 DTG-60/DTG-60H

6.1.6 PID Parameters

Specify the PID constants used for the DTG-60/60H's temperature control. The preset PID
parameters can be changed during measurement. (Normally, the initial values
(factory-settings) need not be changed.)
1. Select the [Detector] menu - [PID Parameters] command.
The "PID Parameter" dialog box is displayed.

2. Enter values between 0 and 10000

3. Select the [OK] button to send the data to the module. The specified PID parameters
will be transmitted to the DTG-60/60H.

The initial values is set as shown in the following table.

P I D
DTG-60 100 100 100
DTG-60H 1000 1000 1000

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DTG-60/DTG-60H

6.2 Troubleshooting

6.2.1 Error codes

The key/display panel displays any of the following error codes according to the error
condition.

ERR error code

Error
Cause Remedy
code
The sample section temperature is above the upper limit
1 value (High temperature type (DTG-60H): 1650°C, Medium
temperature type (DTG-60): 1200°C).
The sample section temperature is below the lower limit
2
value (0°C).
The furnace temperature is above the upper limit value (High
3 temperature type (DTG-60H): 1650°C, Medium temperature
type (DTG-60): 1200°C). Turn off the instrument's
main power supply and
4 The furnace temperature is below lower limit value (0°C).
contact your Shimadzu
The furnace temperature is higher than the sample section representative.
5
temperature by 150 C or more.
The sample section temperature is higher than the furnace
6
temperature by 150 C or more.
The sample section temperature or the furnace temperature
7
never rises.
Although press the [OPEN/CLOSE] key, the furnace lid
8
cannot be normally opened (or closed).

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 DTG-60/DTG-60H

6.2.2 Troubleshooting
WARNING
 In the case of any problems other than those detailed above, our
service staff will need to be consulted.
Please understand that Shimadzu will not take responsibility for any
deterioration of system performance or safety resulting from unauthorized
modification of the system.

Temperature-Related Problems
Symptom Cause Remedy

The circuit board or component must be replaced.

The circuit board or component is
damaged.
Abnormal temperature is
indicated for the ambient
temperature.
There is an abnormal value in the
temperature correction coefficient
Improper temperature control
constants (P, I, D)
The temperature program is
The sample temperature incorrectly configured
does not change even
when the measurement An unintended value is set in [The
starts setting upon starting measurement].
The circuit board or component is
damaged.
The temperature program is not
intended.
Turn off the instrument's main power supply and contact
your Shimadzu representative.
There is an abnormal value in the temperature correction
coefficient.
6.1.1
Change the control constants.
7.1.6
Reconfigure the temperature program using feasible
settings.
Check if an unintended value is set in [The setting upon
starting measurement].
If this does not work, replacements are required. Turn off
the instrument's main power supply and contact your
Shimadzu representative.
Change to a feasible temperature program.

When measurement An unintended value is set in [The
starts, temperature starts setting upon starting measurement].
to rise suddenly.
The circuit board or component is
damaged.
Improper temperature control
constants (P, I, D)
Temperature deviates Poor detector contact,
largely from programmed detector thermocouple wire
temperature (Defective disconnection
temperature control).
Baseline contains
temperature control There is an electromagnetic noise
noise (hunting and source nearby
meandering).
The power supply conditions are
poor.
Temperature does not The circuit board or component is
change damaged.
Check if an unintended value is set in [The setting upon
starting measurement].
The circuit board or component must be replaced.
Turn off the instrument's main power supply and contact
your Shimadzu representative.
Change the control constants.
The detector must be replaced.
Turn off the instrument's main power supply and contact
your Shimadzu representative.
Identify the noise source and implement noise
countermeasures.
Consider changing the install location. (Contact your
Shimadzu representative to request that the unit be
relocated.)
Supply power through a power supply stabilizer.
The circuit board or component must be replaced.
Turn off the instrument's main power supply and contact
your Shimadzu representative.

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DTG-60/DTG-60H
DTA Signal-Related Problems
Symptom Cause
DTA signal remains Poor detector contact, detector
showing maximum or thermocouple wire disconnection
minimum Wire of detector thermocouple is broken. Turn off the instrument's main power supply and contact
Poor detector contact, detector
thermocouple wire disconnection
Heat flow signal
fluctuates largely at the
There is an electromagnetic noise
ambient temperature.
source nearby
Incorrect detector connection
DTA signals deflects to orientation
the wrong side.
The sample is placed on the left side
as viewed from the front
The difference in heat capacity
between the sample and the reference
material is large
The sample container is placed in the
wrong position
The heating speed is too fast
The baseline adjustment parameter
value setting is incorrect
Large baseline drift
Soiled or deteriorated detector or
furnace
Deformed detector
Loose screws, etc.
Sample container bottom is not flat
Dust between detector plate and
sample pan
Soiled or deteriorated detector or
furnace
Deformed detector
The circuit board is damaged
High noise level during
temperature control
Affected by external vibrations
There is an electromagnetic noise
source nearby
The unit is exposed to strong wind or
significant fluctuations in room
temperature
- 42 -
Remedy
The detector must be replaced.
your Shimadzu representative.
Identify the noise source and implement noise
countermeasures. Consider changing the install
location. (Contact your Shimadzu representative to
request that the unit be relocated.)
The detector must be replaced.
Turn off the instrument's main power supply and contact
your Shimadzu representative.
Measure again with the sample placed on the right side.
4.1.3
Adjust the reference material quantity and align the heat
capacities of both.
4.2.3
Place it right about in the middle of the circular detector
area without allowing it to tilt or stick out.
To the extent possible, set the speed to 50 °C/min or less.
Add the parameter value solved from the measurement
result to the original parameter value and reconfigure it
as the new K-value.
7.1.3
• Clean with the appropriate solvent.
• Clean the detector or furnace.
If this does not work, replacements are required. Turn
off the instrument's main power supply and contact your
Shimadzu representative.
7.1.5
The detector must be replaced.
Turn off the instrument's main power supply and contact
your Shimadzu representative.
Inspection and repair are required.
Turn off the instrument's main power supply and contact
your Shimadzu representative.
Make the bottom flat, or replace the pan with a new one
having a flat bottom.
4.2.2
Eliminate dust.
• Clean with the appropriate solvent.
• Clean the detector or furnace.
If this does not work, replacements are required. Turn
off the instrument's main power supply and contact your
Shimadzu representative.
7.1.5
The detector must be replaced.
Turn off the instrument's main power supply and contact
your Shimadzu representative.
The circuit board must be replaced.
Turn off the instrument's main power supply and contact
your Shimadzu representative.
• Install the instrument on a stable stand.
• Implement measures to minimize vibrations.
• Change the install location.
(Contact your Shimadzu representative to request that
the unit be relocated.)
Identify the noise source and implement noise
countermeasures. Consider changing the install
location. (Contact your Shimadzu representative to
request that the unit be relocated.)
• Use a screen, etc. to prevent wind from directly
hitting the unit.
• Install the unit in a location with small temperature
fluctuations.
• Change the install location.
(Contact your Shimadzu representative to request that
the unit be relocated.)
 DTG-60/DTG-60H

Troubles as the TG system

Symptom Cause
The weight signal
The balance is not properly set.
exceeds the range.
The detector contacts with the
furnace wall or the reflective plate.
The detectors touch each other.
Affected by external vibrations
The weight signal
noise is too large. There is an electromagnetic noise
source nearby
The unit is exposed to strong wind
or significant fluctuations in room
temperature
The detector contacts with the
furnace wall or the reflective plate.
The TG curve has no
The detectors touch each other.
reproducibility. Gas purge is defective due to
clogging, leak, or other reason.
An extra increment or
The detector, sample pan is
decrement appears in
dirty.
the TG curve.
The heating rate is too fast
The flow rate of purge gas is too
The TG curve shows fast.
marked drift.
The weight detector is overheated
due to a cooling fan failure.
Remedy
Complete the weight of sample and reference
4.2.3
Change the sample weight less than 1g (in gross
weight).
Inspection and repair are required.
Turn off the instrument's main power supply and contact
your Shimadzu representative.
• Install the instrument on a stable stand.
• Implement measures to minimize vibrations.
• Change the install location.
(Contact your Shimadzu representative to request that the
unit be relocated.)
Identify the noise source and implement noise
countermeasures. Consider changing the install location.
(Contact your Shimadzu representative to request that the
unit be relocated.)
• Use a screen, etc. to prevent wind from directly hitting
the unit.
• Install the unit in a location with small temperature
fluctuations.
• Change the install location.
(Contact your Shimadzu representative to request that the
unit be relocated.)
Inspection and repair are required.
Turn off the instrument's main power supply and contact
your Shimadzu representative.
Clean it with acetone or replace it.
4.2.2
Check the heating rate of purge gas (adjust it to 50℃
/min or less)
Check the flow rate of purge gas (adjust it to
50ml/min or less)
3.4
Inspection and repair are required.
Turn off the instrument's main power supply and contact
your Shimadzu representative.

Noises are heard Identify the noise source and implement noise
There is an electromagnetic noise countermeasures. Consider changing the install location.
when the furnace is source nearby (Contact your Shimadzu representative to request that the
raised or lowered. unit be relocated.)

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DTG-60/DTG-60H

Other troubles
Symptom Cause Remedy
The circuit board or component must be replaced.
Power is not The circuit board or component is
Turn off the instrument's main power supply and contact
supplied. damaged.
your Shimadzu representative.
The LCD unit must be replaced.
The liquid crystal is damaged or reached
Abnormal LCD Turn off the instrument's main power supply and contact
its life span
your Shimadzu representative.
Inspection and repair are required.
The [POWER]
Parts such as LED are out of order Turn off the instrument's main power supply and contact
lamp does not light
your Shimadzu representative.
even when the
power switch is The circuit board or component must be replaced.
The circuit board or component is
pressed. Turn off the instrument's main power supply and contact
damaged.
your Shimadzu representative.
The furnace elevating temperature is set
The furnace is not to a temperature lower than the current Set the temperature higher than the current temperature.
raised nor lowered temperature.
by pressing Inspection and repair are required.
[OPEN/CLOSE] Part failure Turn off the instrument's main power supply and contact
your Shimadzu representative.
Does not stop when
The circuit board must be replaced.
the furnace reaches
The circuit board is damaged Turn off the instrument's main power supply and contact
the highest or
your Shimadzu representative.
lowest point
Abnormal noise is
The furnace must be replaced.
generated when
Malfunction of furnace Turn off the instrument's main power supply and contact
raising and lowering
your Shimadzu representative.
the furnace
Check that the cord is connected to the communication
Poor communication cable connection port on the rear of the unit.
Data
2.2
communication is
not possible. The circuit board or component must be replaced.
The circuit board or component is
Turn off the instrument's main power supply and contact
damaged.
your Shimadzu representative.
Inspection, adjustment, and part replacement is required.
The furnace O-ring is not sealed Turn off the instrument's main power supply and contact
your Shimadzu representative.
The gas pipe is not aligned with the Check the gas piping and make adjustments.
Purge gas is
connection point 3.4
leaking or does not
flow Remove and clean the O-ring if it is contaminated.
Replace the O-ring if it has deteriorated or been damaged.
Packing and O-ring degradation,
If the situation is still not improved, turn off the instrument's
damage, contamination, etc.
main power supply and contact your Shimadzu
representative.

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

CAUTION
Please understand that Shimadzu will not take responsibility for any
deterioration of system performance or safety resulting from unauthorized
modification of the system.

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 DTG-60/DTG-60H

6.3 Maintenance
If the DTG-60/60H is not used for a long period of time, seal it as shown with the nipple MNO
and the nut MF at the gas inlet. Do not place anything on the detectors. Lower the
furnace to prevent any dust from entering the inside. Do not lean the DTG-60/60H, nor
place it upside down. Avoid storing it wherever it is exposed to direct sunlight, hard
vibrations, or a large amount of dust.

Replacement of parts
Be sure to consult our service staff on replacement of heater, detector and other
components. Please understand that Shimadzu will not take responsibility for system
performance deterioration or any accidents resulting from replacement or repair of parts
performed by the customer without our approval.

Storage
When system is to be long out of service, disconnect the gas supply pipes, and close the
respective ports with nipples and nuts. Close the furnace lid then furnace cover securely,
with nothing on the detector plate, and set the cell cover so that dust does not enter the
interior. Do not store the unit inclined or upside down.
For storage, avoid a place exposed to direct sunlight and severe vibration as well as a dusty
place.

6.3.1 Consumables List

Recommended
Part Name Part Number replacement Remarks
frequency
For each
Al pans 201-52943 measurement With lid; 50pcs.in a set
For each
Pt pans 201-51976 measurement
For each
Pt pan lid 201-56927 measurement
For each
Alumina pans 201-54321 measurement
For each
Alumina pan lid 222-13027-91 measurement
For each
α-alumina powder 201-53537 measurement

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DTG-60/DTG-60H

7 Technical Data

7.1 Specifications
Measured temperature range : DTG-60H --- Room temperature to 1,500°C
DTG-60 --- Room temperature to 1,100°C *1)
Balance type : Parallel guide differential top pan type
Supporting point type : X-shaped supporting point
Weight readability : 0.1μg
Measurable range : ±500mg
Measurement accuracy : ±1％
Detector : Thermocouple of platinum plus 10% platinum/rhodium (plug-in type)
Measurable range : ±1 to ±1000µV
Analysis conditions
Heating rate *2) : Setting at 0.1°C/min or 0.1°C/hour increment/decrement
DTG-60H ---
maximum heating rate 50.0°C/min
DTG-60 ---
maximum heating rate up to 800°C : 99.9°C/min
maximum heating rate up to 900°C : 75.0°C/min
maximum heating rate up to 1000°C : 50.0°C/min
maximum heating rate up to 100°C : 25.0°C/min
Atmosphere : Air or inert gas (nitrogen, helium, or argon)
Recommended flow rate:
100 ml/min in air, 300ml/min in inert atmosphere
Sample quantity *3) : 1g max. in gross weight
Sample form : Substance which is solid or liquid qt ambient temperature (A
void measuring a sample possibly evolving toxic exhaust or
generating corrosive degradation products)
Cleaning condition
"Cleaning" gas : Clean air supply at the rate of 200 to 300 ml/min required in
order to bake and clean up the furnace/detector.
On/off control with the built-in solenoid value.
Installation conditions*4) *5)
Power supply : 100V AC or 120V AC or 220,230,240V AC ±10%, 50/60Hz
Current capacity : DTG-60H --- 1500VA or larger, DTG-60 --- 1300VA or larger
Breaking capacity of the fuse : 35A
Ambient temperature : 5 to 40C ( Humidity : 80% or less)
Dimensions : About 367 mm(W) × 650 mm (D) × 474 mm (H)
Weight : About 35 kg
*1) When you want to measure more than 1000°C with the DTG-60 and more than 1300°C with the DTG-60H,
you set hold time less than 5 minutes. Otherwise, temperature of a heating furnace cover rises unusually
and is fear to cause a scald, if it touches them. And, life span of heater of furnace gets short.
*2) There are cases where these specifications will not be satisfied due to the installation environment such as
supply voltage.
*3) For details about sample pan weight and capacities, refer to 4.2.1.
*4) So-called "stand-alone" operation of the DTG-60/60H is impossible. Always use it connected with the
TA-60WS system. To control the DTG-60/60H, TA-60WS（Ver. 1.40 or greater) or LabSolutionsTA is
required.
*5) Install the instrument in an indoor location under the following classifications: installation category II, pollution
level 2, and altitude 2,000 meters max.

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 DTG-60/DTG-60H

7.2 Principle & Construction

7.2.1 Principle of measurement by DTG-60/60H

When the sample and the reference substance are heated at a constant rate, their
temperatures increase as shown in Fig. 7.1 using a dashed line and a one-dot chain line,
respectively. Since the reference substance is thermally inert, its temperature continues to
show a stable increase. If any endothermic change (for example, fusion) has occurred in
the sample, the externally applied heat energy will be consumed for that reaction and thus
the temperature increase is hindered. When the change is over, the occurrence of a great
temperature difference from the ambient temperature causes a large quantity of heat energy
to enter the sample. This suddenly increases the temperature, brings the sample back to
its original state, and then makes the temperature start increasing again at a stable rate.
Now, if the temperature difference between the two (hereinafter referred to as "DTA signal")
is detected and then amplified, it can be recorded as the signal of peak shown with a solid lie
in Fig. 7.1.

Fig. 7.1 Typical DTA curve

The sample temperature (furnace temperature) is measured with a thermocouple for

temperature sensor. After each signal is managed with an electric circuit inside this
equipment, regulate a voltage to take part in a heater of furnace by comparing a temperature
program and an actual temperature set up by a built-in microcomputer. The sample
temperature is digitally shown on the readout located on the front panel and simultaneously
stored in the PC via TA-60WS interface as a digital data.

The DTG-60/60H can use the temperature signals on the furnace as temperature control
signals in order to obtain a stable base line. The temperature reading shown on the
readout and the PC is the one obtained from the sample detector. (By a change of a set up,
you can control a temperature depending on sample temperature. Refer to 4.5)
The weight detection unit for the DTG-60/60H uses the parallel guide mechanism. When
connection rods AA' and BB' with the same length are used to connect two levers which
have supporting points at F and F' in Fig. 7.2, AA'B'B, AA'F'F, and FF'B'B from
parallelograms. Now if arms C and C' are presumed to exist on AA' and BB', applying load
to those arms at whatever points will result in applying load point to A or B.

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DTG-60/DTG-60H

The load does not change depending on the loading positions. This mechanism is called
the parallel guide mechanism. The DTG-60/60H uses the structure where the portions
equivalent to arms C and C' are extended above point A or B and then horizontally extended
toward supporting point F. For lever A'F'B', a wire is used and for A'F', another wire is used.
Thus, the parallel guide mechanism similar to that shown in the operation principle diagram
is structured (see Fig. 7.3). This structure assures a constant sensitivity of the balance
wherever the sample is positioned on the sample pan. In addition, since the mechanism is
a differential type, it offers the advantages that the sensitivity is less influenced by buoyancy
and the flow rate of gas, and that the drift is smaller when the sample temperature is
changed.

Fig. 7.2 Fig. 7.3

The figure 8.4 is the object to show a principal portion of a weight detection division of this
equipment. Usually, when the reference sample is placed on the left side and the sample
on the right side to balance the beam, the sample weight changes if the sample temperature
is increased.
Then, beam AFB rotates around supporting point F and show inclination. Now the shutter
located at the center of the beam similarly rotates, which result in a change in the quantity of
light coming from the lamp to the photoelectric conversion element. This change is
amplified to flow current in the coil placed in the magnetic field. Thus, the rotational
moment equivalent to the change in the sample weight is generated to bring the beam back
to its original position instantaneously. This method of maintaining the beam in place is
called the null method. The rotational moment is directly proportional to the value of electric
current, which generates it. If this relation is calibrated in the moment weight and the value
of electric current, the changes in the sample weight can be continuously and accurately
measured from those in the value of electric current.

Fig. 7.4

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 DTG-60/DTG-60H

7.2.2 Standard materials used for calibration of DTA

apparatuses

Standard material Transition Enthalpy of fusion NIST catalogue number

temperature in C in J･g-1
Cyclohexane -83* NIST RM 8757
Mercury -38.85 11.469 NIST SRM 2225
1,2-Dichloromethane -32* NIST RM 8757
Cyclohexane 7* NIST RM 8757
Phenyl ether 30* NIST RM 8757
0-Terphenyl 58* NIST RM 8757
Biphenyl (99.984%) 69.26 120.41 NIST SRM 2222
Potassium nitrate 127.7 NIST RM 8758
Indium 157 28.42 NIST RM 8758
Tin (99.9995%) 231.95 60.22 NIST SRM 2220
Tin 232 NIST RM 8758
Potassium 299.5 NIST RM 8758/8759
perchlorate
Lead 327.5 23.16
Zinc (99.999%) 419.59 107.46 NIST SRM 2221a
Silver sulfate 430 NIST RM 8758/8759
Quarts 573 NIST RM 8759/8760
Potassium sulfate 583 NIST RM 8759/8760
Potassium chromate 665 NIST RM 8759/8760
Barium carbonate 810 NIST RM 8760
Strontium carbonate 925 NIST RM 8760

The values in boldface indicate temperatures/enthalpies of melting.

The values with an asterisk indicate DSC/DTA peak temperatures, and the others
indicate equilibrium transition temperatures, respectively.
For details, refer to "http://ois.nist.gov/srmcatalog/index.cfm".

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