Standard Operating Procedure

Thermogravimetric Analyzer (TGA) & Differential Scanning

Calorimeter (DSC) – TA Instruments DSC SDT Q600

The SDT Q600 is an instrument capable of making two different thermal analysis measurements
simultaneously on the same sample. Depending on which operational mode is used, these
measurements are heat flow (DSC) and weight change (TGA) or differential thermal analysis
(DTA) and weight change (TGA). Simultaneous measurement of two properties not only
improves productivity but also simplifies interpretation of results. The information provided
allows differentiation between thermal events that have no associated weight change (e.g.,
melting, phase change) and those which involve a weight change (e.g., decomposition).

1.0 Operation Procedure

NOTE: Please come to discuss with the MCL staff before you starts to use a
new sample material in this instrument. All the physical and chemical
properties of this new sample material must be reviewed and discussed!!!
Electrical Safety
 You must unplug the instrument before doing any maintenance or repair work. Voltages
exceeding 120 volts AC are present in this system. If you are not trained in electrical
procedures, do not remove the cabinet covers unless specifically instructed to do so in
the manual.
 After transport or storage in humid conditions, this equipment could fail to meet all the
safety requirements of the safety standards. The equipment needs to be dried out
before use.

Chemical Safety
 Use only the purge gases listed in manual. Use of other gases could cause damage to the
instrument or injury to the operator.
 Do not use hydrogen or any corrosive or flammable gases in the SDT furnace. Air can be
used as a purge gas in the SDT. However, the furnace must be kept clean of volatile
hydrocarbons that might combust.
 The SDT furnace assembly contains a layer of refractory ceramic fiber (RCF) insulation.
This insulation is completely encapsulated within the furnace can, which is not meant to
be disassembled.
 If you are using samples that may emit harmful gases, vent the gases by placing the SDT
near an exhaust.

Thermal Safety
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 After running an experiment, allow the open furnace and sample beams to cool down
before you touch them.
 During a sample run, the furnace can be hot enough to burn skin. Avoid contact with the
furnace during experiments.

Mechanical Safety
 Keep your fingers and all other objects out of the path of the furnace when it is moving.
The furnace seal is very tight.
 The SDT is a fairly heavy instrument. In order to avoid injury, particularly to the back,
please use two people to lift and/or carry the instrument. The instrument is too heavy
for one person to handle safely.

1.1 Create a Method

a. Open the purge gas valves, 100 kPa N2
b. Double-click “TA Instrument Explorer” icon on the desktop
c. Double-click “Q600-0671” in TA Instrument Explorer window to launch the control
software
d. Select Experiment View and access the Summary Page
e. Select “SDT Standard” from the Mode list
f. Select “Custom” from the Test list
g. Enter the Sample Name
h. Select the appropriate Pan Type (Alumina, Platinum, or Other for aluminum pans)
i. Specify a Data File Name using the browse button
j. Click on the Procedure Page
k. Enter the Method Name
l. Click on the Editor button
m. Create a method by double-clicking the command in the Segment List. For example:
#1 Sample interval: 0.5 sec / pt
#2 Data Storage: Off
#3 Equilibrate at 250.00 °C
#4 Data Storage: On
#5 Ramp 20.00 °C/min to 500.00 °C
n. Click on the Advance button to access and select the Advanced Parameters
o. Click on the Post button to access the Post Test Parameters that allow you to
specify the furnace and air cool options to use once the experiment is complete
(select “Furnace Closed” and Air Cool to 25°C)
p. Click on the Notes Page
q. Enter the Operator name, select “#1 - Nitrogen” in Mass Flow Control Settings, and
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specify the Flow Rate to be 100 mL/min

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 r. Click on Apply to store the changes made to these pages

1.2 Start the Experiment

a. Click Control  Furnace  Open to open the furnace
b. Remove all SDT pans, samples and weights from the sample and reference beams
c. Obtain two clean, empty 90 µL alumina pans (or other pan type) and then position
them on the platforms. Position the pans as close as possible to the beam side of
the sensor.
d. Click Control  Furnace  Close to close the furnace
e. Once the balance has stabilized, click Calibrate  Tare, and wait for the readings of
Weight and Reference Weight to stabilize again
f. Click Control  Furnace  Open to open the furnace again
g. Place about 2 to 20 mg samples into the sample pan, and replace it on the SDT
sample (front) platform. Position the sample pan as close as possible to the
previous position.
h. Click Control  Furnace  Close to close the furnace
i. Click the “Start the Run” button (green) to begin the experiment

1.3 After the Experiment

a. After the experiment is completed, an error message may appear like below. Click
OK to acknowledge it.
b. Click Tools  Data Transfer to transfer data file from the instrument to controller
c. Specify the Data Path using the browse button, then click Transfer
d. Wait for the DFA Status to show “The data file receiving completed”, then click
Close
e. Find your saved data file in the folder named “Shortcut to TGA-DSC Results” on the
desktop. The data file can be opened by the TA Universal Analysis software.
f. Wait for the furnace temperature to be below 25 °C, then open the furnace
g. Remove all SDT pans, samples and weights from the sample and reference beams
h. Close the furnace
i. Close the control software
j. Close the purge gas valves
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2.0 Specifications/Features
 Sample capacity: 200 mg (350 mg including sample holder)
 Balance sensitivity: 0.1 µg
 Calorimetric accuracy: ±2% (based on metal standards)
 Furnace type bifilar wound
 Temperature range: up to 1300 ºC
 Platinum thermocouple beams
 Heating rate: 80 ºC/min for < 1000 ºC; 20 ºC/min for 1000-1300 ºC
 Furnace cooling forced air: 1300 ºC to 50 ºC in ~30 min
 Sample pans: 110 µL Pt, 90 µL Al2O3
 Brand new Al2O3 sample pans for sale
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3.0 User Requirements

The TA Instruments SDT Q600 TGA-DSC must be used by authorized personnel only. All
authorized users are expected to read and understand this SOP and follow the operation
instructions carefully. No unauthorized user may operate this TGA-DSC unless accompanied by
an authorized user. All visitors must be briefed on proper safety protocol and must wear
appropriate personal protective equipment. To become an authorized user, one must:

1. Complete Environment, Health & Safety (EH&S) training

2. Complete initial orientation and training for the Materials Characterization Laboratory
3. Receive training on this piece of equipment from lab personnel
4. Schedule equipment time using the calendar
5. Read and fully understand this SOP

4.0 General Safety

4.1 Required Personal Protective Equipment

Users must wear lab coats, safety glasses, and gloves. Shorts, open-toed shoes, high
heels, and skirts, are forbidden.

4.2 Emergency Procedures and Contacts

For non-life threatening emergencies: notify the MCL facility manager and your PI
immediately.
Facility manager: Zongmin (Shirley) Bei, Ph.D.
Office: 109B Furnas Hall, Tel: (716) 645-5165, Cell: (585) 354-5623
Email: zongminb@buffalo.edu
or for police / ambulance, call 645-2222

In case of fire or other life threatening emergency: Exit the laboratory through an
emergency exit door. Pull one of the fire alarms located in the main hallway. Dial
campus police / ambulance at 645-2222.

4.3 University after hours laboratory use policy

No working alone, use the buddy system!

# Revised by Date Modification

1 Zongmin (Shirley) Bei 04/22/2016 Document initial release
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