Differential Scanning Calorimeter

GT-DSC-300

Operation
Instructions

1
 Directory
1. Instrument Introduction ____________________________________ 1

2. Instrument principle _______________________________________ 2

3. Instrument characteristics __________________________________ 4

4. Instrument interface _______________________________________ 5

5. Software description ______________________________________ 7

6. Selection of calibration items: ______________________________ 24

7. Instrument application ____________________________________ 25

8.Notes for instrument use ___________________________________ 28

9.Bating list ______________________________________________ 31

2
1. Instrument Introduction
The Differential scanning calorimetry (DSC) technique has been widely
used. The differential scanning calorimeter is both a routine quality test
tool and a research tool. Measmeasures the temperature, heat flow
associated with the thermal transition inside the material. Our
instrument is a heat flow type differential scanning calorimeter, with
good repetition and high accuracy, which is especially suitable for
accurate measurement of specific heat. The equipment is easy to calibrate,
uses a low melting point, is fast and reliable, and has a very wide range
of applications, especially in material research and development,
performance testing and quality control. The properties of materials,
such as glass transition temperature, cold crystallization, phase
transition, melting, crystallization, product stability, curing /
crosslinking, oxidation induction period, etc., are the research fields
of differential scanning calorimetry, and different models are selected
according to the experimental parameters and experimental requirements.

The application scope of differential scanning calorimeter is:

curing reaction temperature and thermal effect of polymer materials,
material phase transition temperature and thermal effect measurement,
crystallization of polymer materials, melting temperature and
thermal effect measurement, glass transition temperature of polymer
materials, etc.

The sample and parameters were placed into the crucible separately
and placed in the furnace for programmed heating to change the temperature
of the sample and parameters. If the heat capacity of the reference and
the sample are the same, and the sample has no heat effect, the temperature
difference is almost "zero", and a smooth curve is obtained. As the
temperature increases, the sample has a thermal effect, and the parameter
does not produce a thermal effect, the temperature difference between the
two, in the DSC curve, the larger the temperature difference, the greater
the temperature difference changes, the more the number of peaks. Peak

1
up are called exothermic and peaks down are called heat absorption.

The following figure is a typical DSC curve showing four types of

transitions:

ⅠFor a secondary transition, it is a change in

the horizontal baseline
Ⅱ For the heat absorption peak, it is caused by
the melting or melting transition of the test sample
Ⅲ For the heat absorption peak, it is caused by
the decomposition or cleavage reaction of the test
sample

Ⅳ is the exothermal peak, which is the result of the

sample crystalline phase transition

2. Instrument principle
Material is often accompanied by thermal effects during physical and
chemical changes, and heat release and heat absorption reflect the thermal
enthalpy of matter. A differential heat analyzer is a function of
measuring the temperature or time between the test sample and the
reference under the same thermal condition.

Differential scanning calorimetry is a technique to measure the power

difference between the output material and the parameter under a
program-controlled temperature. The instrument of our company is the heat
flow type differential scanning calorimeter, with the thermal flow
difference between the sample and the parameter in mw. The abscissa is
time (t) or temperature (T), increasing from left to right (not meeting
this requirement shall be noted).

After the sample and the reference are put into the crucible, they
heat up at a certain rate. If the thermal capacity of the reference and
the sample is roughly the same, the ideal scanning calorimetric analysis

2
map can be obtained.

The figure T is the temperature curve reflected by the thermocouple

interpolated in the reference. Temperature difference curve between the
AH-line reaction sample and the reference. If the sample had no thermal
effect, then the △T=0 between the sample and the reference showed a
baseline as smooth as the AB, DE, GH on the curve. When the temperature
of the sample occurs below the temperature of the sample of the parameter.
Conversely, peak-up EFG exothermic peaks appear.

The number of peaks, location, peak area, direction, height, width,

symmetry in the figure reflects the physical and chemical changes of the
sample in the measured temperature range, the temperature range of the
transition, thermal effect magnitude and positive and negative. The
height, width, and symmetry of the peaks, in addition to the test
conditions, the dynamics in the sample change, and the measured results
are much more complex than the ideal curve.

3
3. Instrument characteristics
1.New furnace structure, better resolution, resolution and baseline
stability.

2.instrument offline computer data real-time transmission, interface

friendly, easy to operate.

DSC GT-DSC-300 Differential scanning calorimeter

DSC range 0~±600mW
Temperature
room temperature~ 500℃
range
Heat-up rate 0.1~100℃/min
Temperature
0.001℃
resolution
Temperature
±0.001℃
fluctuations
Temperature
±0.1℃
reproducibility
DSC accuracy 0.001mW
DSC sensitivity 0.01uW
Temperature Heating up and constant temperature (automatic
control method control of the whole program)
Curve scan Heating up the scan
Air control The instrument switches automatically
The 24bit color 7-inch LCD touchscreen display
Display mode
is shown
Data interface Standard USB interface
Instrument Equipped with standard substances (Sn), the user
standards can correct the temperature and thermal enthalpy
All technical indicators can be adjusted
Note
according to the user needs

4
4. Instrument interface

4.1 Instrument Interface

4.1.1 The Initial Status key is used to view the ambient temperature,
sample temperature, etc.

4.1.2 The Parameter Settings key is used to set the experimental

parameters, generally on the software.

5
4.1.3 The Device Information key displays the device information. The
administrator channel is used for the internal personnel calibration
temperature.

4.1.4 The Start Run key to display the current data information after
the operation on the computer software.

6
5. Software description

5.1 Open the software, click [New] or [New] shortcut under the menu bar

in the figure below:

5.2 After clicking "new", you will transfer to a new window, in the new

window, enter [sample name], [sample quality], [operator], [experimental

parameters], [atmosphere] and other information, test type choose [OIT]

or [Not OIT] according to customer needs, click [connected instrument],

and you will hear a beep.Note two experiments, the sample name can not

be the same, otherwise the last data, resulting in the loss of the last data.as

illustrated in following figure:

7
The experimental parameters are set as follows:
5.2.1 "Parameter setting of oxidation induction period experiment" as
shown in the figure: (Stage 1 can choose constant temperature time 5-10
minutes, scanning rate 20, the end temperature is 190-210℃, commonly used
as 200℃.Phase 2 scanning rate 0, the end temperature is the same as phase
1, the time should be greater than the sample OIT time of more than 10
minutes.When the sample time is unknown, it can be set to 150 or
200min.Test Type Selection OIT)

Software with OIT automatic analysis function, check the OIT

automatic analysis mode, OIT automatic analysis parameters, operation
steps and analysis parameters set as follows:

8
 After selecting the automatic mode, the instrument

automatically stops the experiment after the software detects

the oxidative exothermic peak, and calculates the data to

obtain the OIT time.

5.2.2 "Parameter setting of melting point and phase change temperature

experiment" (according to the sample estimated parameter setting, the
test type, select Not OIT.) as illustrated in following figure:

9
5.2.3 "Parameter setting of two or more section lifting temperature"
(select Not OIT according to the estimated parameter setting of the
sample.) as illustrated in following figure:

5.2.4 "Parameter setting of specific heat capacity experiment" (select

not-OIT according to the test type.) as illustrated in following figure:

10
11
5.3 After the software setting is complete, click [Connect

instrument] and start key " " in the upper left corner of the

software (the figure below). The device will heat up according

to the set program, and the software will record the data in

real time.At the set temperature, the instrument stops

automatically and the following map appears (the melting point

and phase change temperature map)

5.4 First, save the map first to prevent loss. You can also use

the shortcut key to select [Save as a sample].The analysis was

12
followed by the following analysis.as illustrated in following

figure:

5.4.1 Melting point, heat enthalpy, phase change temperature analysis

process: click the map to make it green, that is, selected map, click the
task bar [analysis] - [peak comprehensive analysis] -appear about two
black lines, drag the left analysis line in the front, the right analysis
line in the back end, select, click [application], [sure], then click the
curve, make it blue, analysis.The analyzed map is shown below:

13
5.4.2 Oxidation induction analysis process: click the map to make it green,
that is, the selected map, click [] - [analysis in the oxidation induction
period] -about two black lines, drag the left analysis line in the front,
the right analysis line in the back end, after selection, click
[application], [sure], then click the curve, make it rose red,
analysis.The analyzed maps are shown in the figure below

14
15
Software OIT automatic analysis function, the instrument operation is finished,
directly appears in the following figure:

5.4.3 Glass analysis operation: click the map to make it green, that is,
select the map, click [analysis] - [glass transformation] in the
taskbar-about two black lines, drag the left analysis line in the front,
the right analysis line in the back end, select, click [application],
[sure], then click the curve, make it blue, analysis.The analyzed maps
are shown in the figure below

16
17
5.4.4 Initial melting point, final melting point analysis: click the map
to make it green, that is, selected map, click the task bar [analysis]
- [initial melting point] or [final melting point] -appear about two black
lines, drag the left analysis line in the front, right analysis line in
the back end, select, click [application], [sure], then click the curve,
make it blue, analysis.The analyzed map is shown below:

18
19
5.4.5 Specific heat capacity analysis: open the three maps of the test,
click the map to make it green, that is, select the map, right click, select
the corresponding items (baseline, standard sample, sample), click
[Analysis] - - [specific heat-specific heat method] in the task bar-
-enter the temperature to be compared-click calculation. The analyzed map
is shown as follows below:

20
21
5.5 For all analyzed maps, click [File] - [Save as status T]

to save the analyzed data.as illustrated in following figure:

5.6 All maps can be reported, click [print preview], as shown

below:

22
Operation procedure for temperature calibration:
1、 Enter "456" in the administrator channel, click input, and enter the temperature correction
interface. The following below:

23
2, at the correction point 2, you can input the corresponding melting point value of indium; the
correction point 3, input the corresponding melting point value of tin, click Save. Note that
correction point 3 needs to be higher than correction point 2. The following below:

6. Selection of calibration items:

Regular temperature correction to ensure test accuracy.
Calicalibration were selected based on the actual test temperature of the
sample. Principles of calibration selection: the extrapolation
temperature of the calibration should be close to the temperature of the
sample items to be tested to ensure the accuracy of the test. Our company
only offers the tin calibration.

The following table shows the melting points and theoretical thermal
enthalpy values of the commonly used calibration.

24
 Theoretical
Standard Theoretical
enthalpy of melting
substances melting point, ℃
heat is J/g
Inum In 156.6 28.6
Tin Xi 231.9 60.5
Zinc-based Zn 419.5 107.5

7. Instrument application

7.1 Melting point (thermal enthalpy) measurement

The melting point is the transition temperature of matter from

crystalline phase to liquid phase, which is one of the most common physical
data measured by thermal analysis.The error of its measured accuracy and
the thermodynamic equilibrium temperature can reach about ± 1 ℃.At
present, the method recommended by ICTA is used to measure the melting
and heat absorption bee of a certain solid material.In the figure below,
the B 'corresponding to point B is the starting temperature Ti, and the
temperature corresponding to point G is the extrapolated start
temperature Teo, that is, the intersection of the tangent at the maximum
slope of the peak and the intersection of the front baseline extension,
the temperature corresponding to point C is the bee top temperature Tm,
and the D' corresponding to point D is the termination temperature Tf.

25
 Thermal enthalpy is a state function of the energy of a matter system
that is numerically equal to the product of its internal energy U plus
pressure P and volume V, namely H=U + PV.Under certain conditions, the
internal energy and enthalpy changes can be measured from the heat
transfer between the system and the environment.In the absence of other
work, all the heat absorbed by the system in the isovolume process is used
to increase the internal energy, and all the heat absorbed by the system
in the isotropic process is used to increase the enthalpy. Because the
general chemical reactions are mostly carried out under the isovoltage,
the enthalpy is of more practical value.In the DSC curve, we can obtain
the melting heat enthalpy of the sample by calculating the peak area,
namely the BCD in Fig.

7.2 Determination of the instrument coefficient

Since the instrument coefficient may change according to the

environment, the temperature, humidity, and so on will have large or small
effects on it.To ensure the accuracy of the experimental results, the
coefficient of the instrument should be measured.Usually, tin, zinc,
indium and so on are used to calibrate the instrument, measuring the
instrument coefficient.

The instrument coefficient is to test the thermal enthalpy of the

calibration object, and then to calculate the theoretical thermal
enthalpy of the calibration object and the calculation formula of the
instrument coefficient.

In the [Data Analysis] column, select the [instrument coefficient]

to appear in the dialog box below, fill the theoretical melting heat
enthalpy and the measured melting heat enthalpy into the corresponding
column respectively, and click the calculation button to get the
instrument coefficient.The instrument coefficient is also used when
calculating the crystallinity. Without continuous experiments, the
instrument coefficient needs to be recorded for future use.

Taking the pure tin sample experiment as an example, the theoretical

thermal enthalpy of the input tin is 60.5J/g, the measured thermal
enthalpy is 36.2251J/g, and the calculated instrument coefficient K is
60.5/36.2251. The instrument coefficient is automatically generated on
the software interface.

Usually the determination of instrument coefficients can be measured

after instrument correction.When the instrument correction is made, the
quality of the standard material is weighed and filled in the mass column

26
in the real-time data column. If the measured phase change temperature
is close to the actual temperature of the sample, the thermal enthalpy
value can be recorded and the instrument coefficient can be calculated
as the coefficient of the instrument.Set the following figure:

7.3 Measurement of the glass transition temperature

Glrification is the process of transforming a substance into a glassy

amorphous form (glass), a state between liquid and solid states in which
no crystal structure exists. DSC determination of glass transition
temperature Tg is based on the fact that the glass temperature transition
increases this property. On the DSC curve, it moves the baseline during
the transition temperature through glass. As shown in Figure 5.1. The A
point in Fig is the point starting to deviate from baseline. Extending
the baseline before and after the transition, the vertical distance △
J between the two lines is called the order difference, and the C point
can be found at △J/2. The tangent from point C intersects the former
baseline extension at point B. ICTA recommends using the B point as a glass
transition temperature Tg. The glass transition temperature, not having
a very fixed value, lives to change with the measurement method and

27
conditions. Therefore, when marking the glass transition temperature of
a certain polymer, the measured method and conditions shall be indicated.

Other phase change temperatures, such as curing temperature,

crystallization temperature, can analyze the same melting point.

8.Notes for instrument use

1. In order to ensure the normal use of the instrument, the sample
shall not undergo thermal decomposition within the test temperature range,
react with metal aluminum and have no corrosion. If the measured sample
produces a large amount of gas during heating up or can cause explosion,
the instrument shall not be used. Therefore, we should have a general
understanding of the nature of the sample before testing.

2. Check whether all connections of the instrument are correct,

whether the gas used is sufficient and whether the tools are complete.

3. In the test, if the aluminum crucible is selected as the sample

28
dish, the maximum temperature of the test shall not exceed 550 ℃.

4. The accuracy and repeatability of the experimental results are high

when the laboratory room temperature is controlled at 20 ℃ - 30 ℃ and
the temperature is relatively constant. When the room temperature is high,
the air conditioner needs to be turned on to ensure that the ambient
temperature is relatively constant in a short time. After each experiment,
the second experiment can be carried out only when the temperature is below
40 degrees.

5. The crucible bottom shall be flat without saw-tooth or bending,

otherwise the heat transfer is poor.

6. When preparing DSC samples, do not sprinkle the samples on the edge
of the crucible to avoid polluting the sensor and damaging the instrument.
The bottom and all external surfaces of the crucible shall be free of
samples and impurities to avoid affecting the experimental results.

7. The amount of sample should be appropriate, neither too much nor

too little. Solid samples are generally about 10mg. The liquid sample
shall not exceed one third of the capacity of the crucible. If the sample
dosage is otherwise required, the dosage shall be determined according
to the requirements.

8. Inorganic samples can be ground and screened in advance; Polymer

samples shall be as uniform as possible; The fiber can be made into the
same length of 1 ~ 2mm; The powdered sample shall be compacted.

9. The crucible shall be placed at a fixed position in the sensor.

When the amount of sample is small, it shall be evenly spread at the bottom
of the crucible and not stacked on one side; If the sample is granular,
it needs to be placed in the center of the crucible.

10. The heating rate is generally 10 ℃ / min. If it is too large,

the curve will drift and reduce the resolution; Too small, long
measurement time.

29
 11. Do not use hard objects to clean the sample holder and test area,
so as to avoid irreversible damage to the instrument.

12. If there is dust or other powdery sundries in the experimental

area, use an ear washing ball to blow it clean, and be careful to blow
it with your mouth to confuse your eyes.

13. During data collection, avoid obvious vibration around the

instrument. It is strictly prohibited to open the upper cover. Slight
collision with the front of the instrument will produce obvious peaks and
valleys on the DSC curve.

14. do not adjust the flow of purified gas in the process of collecting
data, because the slight change of gas flow will affect the DSC curve.

15. After the experiment, be careful of the furnace cover of DSC. When
the temperature drops below 100 ℃, handle it gently with tweezers to
avoid scalding or damage to the furnace cover.

16. Power supply: AC220V, 50Hz, power consumption ≤ 2000W.

17. Disconnect the data cable and close the software before closing
the instrument. To prevent online and communication errors（ This problem
can be found in XP and SP3 systems (other systems have not been tested).

Solution:

1. If the connection is successful and no data is returned, you need to

restart the computer.
2. If you encounter online failure, you need to uninstall the USB device
with exclamation mark in the device manager and reload it without
restarting the computer.

30
9.Bating list

Host 1

The U disk 1

Data line 2

Power cord 1

The Aluminum
200
Crucible

Metal cover 3

Raw adhesive tape 1

Pure tin grains 1 Bag

10A Fuses 5

Sample spoon / sample bar

One for each one
/ tweezers

Eear ball 1

Thracheal 2

Instructions 1

Warranty form 1

Certificate of
1
qualification

Note: If other parts are required, discuss separately

31
 产品保修卡
Product Warranty Card

用户资料 User Information

单位或个人名称 name：_________________________
详细地址 Address：______________________________

______________________________

电话 Tel： _________ 传真 Fax：_________ 邮编 P.C.：________

维修服务记录
Repair Service Record

产品名
产品型号 产品编号
称
Model Product No.
Product
发票号 购买日期 免费保修期
12 个月
Invoice Date of Period of
12Months
No. purchase Warranty
日期 记录 维修人
Date Description Serviced by

32
 User Instructions
In order to ensure the user interests, I have established a quality

assurance system with free warranty service with the card.

Please out the user profile items in the 1. Product Warranty

Card.

2. charging method: free repair during the warranty period,

over the warranty period of repair fee (cost only charge),

to provide lifetime maintenance service for our products.

Collect fees for human damage for improper use.

33