Documenti di Didattica
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sample preparation, evaluation and
interpretation of the resulting curves.
Powerful sensor-furnace combi-
The NETZSCH 360° view for polymer
··
nation for fast heating/cooling
characterization takes this into
account, streamlining operational Outstanding sensitivity and
processes while simultaneously excellent reproducibility
simplifying them.
Unique
Concavus Pans
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High-performance pans for
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excellent reproducibility
3in1 Box for organized
storage
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n Reaction temperatures and
enthalpies Clever and unique SampleCutter,
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n Cross-linking reactions (curing) especially for brittle materials
n Degree of curing
Comprehensive sample
n Specific heat capacity
preparation set
n Distribution of molecular weight
(peak shape), etc.
2
Smart
Measurement
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Simplified user interface
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Automated measurement
AutoCalibration
AutoEvaluation
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Automatic analyses of
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unknown DSC curves
User-independent analysis
Innovative
Identification
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Data-based test
··
interpretation
Open for users'
own data
3
DSC 214 Polyma − The New Benchmark in Cell Design
1
Arena Furnace Corona
2 Sensor 3
Concavus Pans
Its oval geometry drastically This fast-responding sensor is The unique geometry of this
reduces the furnace mass, unmatched in both reproducibil- sample pan features a concave
resulting in faster heating and ity and robustness. bottom. In combination with a
cooling rates. The double- flat sensor, it provides a ring-
symmetric design also leads to an shaped contact zone that is
even temperature distribution. always clearly defined.
IN
ST
R
U
M
EN
T
4
ME
DSC/mW
exo
35
30 Peak Height:
35.08 mW
25
Peak Width
20 at 50% Height:
0.33 K
15
10
0
152 154 156 159 160 162 164
Temperature/°C
DSC measurement on indium (7.3 mg)
The DSC 214 Polyma sets new The ideal combination of the low
standards, incorporating the premium thermal mass Arena furnace with the
Arena furnace in combination with a fast-responding Corona sensor allows
perfectly matched sensor and pan. This for high heating and cooling rates of
unique solution achieves excellent up to 500 K/min − values unachiev-
sensitivity and resolution at the same able with common heat-flux DSCs on
time, which is reflected in the peak the market. Its high reproducibility and
height-to-width ratio. Only in this way robustness are the hallmarks of the
is it possible to detect weak effects and Corona sensor.
separate overlapping ones.
The Concavus pans − in combination
The peak height-to-width ratio, with a flat sensor − always yield a New Furnace, Sensor and Pan
Combination
····
called the Indium Response Ratio, uniform ring-shaped contact zone.
is generally used to characterize These premium pans are specially
Fast heating and cooling rates
the separation capability of a DSC. designed to align to the shape of the
··
The DSC 214 Polyma generates an Corona sensor, resulting in unmatched Excellent reproducibility
Indium Response Ratio of more than reproducibility. In addition, the Unmatched indium
100 mW/°C, a unique number for Concavus pans are subjected to a response ratio
heat-flux DSC systems. careful cleaning process prior to
delivery, which eliminates any Technical key data for the instrument can be
contamination. found on page 23
5
New Ideas To Get Started
SA M
PLE
PREPA
RAT
ION
PAN
6
S
3in1 Box − The Clever Solution for
Transport, Sampling and Archiving
Even the transport and storage of the and providing a fully functional
Concavus pans is consistent with archiving system. The integrated
their premium quality, thanks to the sample register including name
3in1 Box: 96 pans and lids are and mass makes it easy to locate
packaged in an anti-static box retained samples.
divided into 96 separate compart-
ments. This elaborate packing The Concavus pans are actually
prevents deformation of the pans also compatible with common
while allowing easy access to them heat-flux DSCs.
Tray supports a defined sample position
Sample Preparation
··
SampleCutter
New 3in1 Box for easy
withdrawal, storage and
practical archiving
7
DSC 214 Polyma − Opens the Window for Flexibility
Epic Versatility
IN
ST
R
U
M
EN
T
8
ME
High Sample Throughput
Compressed air cooling Closed-loop intracooler IC40 Closed-loop intracooler IC70 Liquid nitrogen cooling system
(RT to 600°C) (-40°C to 600°C) (-70°C to 600°C) (-170°C to 600°C)
9
The Proteus® Software Ushers In a New Era
The novel, greatly simplified user interface of the Proteus® measurement software
reflects a true "intuitive design" concept. There's no need to be an expert in
thermal analysis to start test runs with the DSC 214 Polyma.
NT
ME
AS
UR
E
M
EN
New simplified user interface for measurement definition − predefined methods are activated
T
10
EV
ExpertMode − Not Just for AutoCalibration Allows for
Professional Users Full Concentration on the SmartMode and ExpertMode
··
test procedures
setting or for method definition, state. Calibration procedures, however,
switching from SmartMode over to should be simple, fast and − ideally − AutoCalibration
ExpertMode is the answer. Here, the done along the way.
user has access to the established
Proteus® software functionality, The solution is AutoCalibration. This
including dozens of features and all feature provides automatic creation
adjustment settings. routines for all relevant calibration
curves, automatically loading the
current calibrations while taking the
selected measurement conditions
into account and checking their
validity periods.
11
AutoEvaluation − The First Truly Automatic Evaluation Routine
EN T
EV
AL
UA
T
IO
N
12
IDEN
DSC/(mW/mg)
1.0 exo
0.8
0.6
0.4
0.2
0.0
-0,2
DSC/(mW/mg)
1.0 exo
0.8
Area: 401.0 J/g
Peak: 251.2°C
0.6
Mid: 747.5°C
0.4 Delta Cp*: 0.33 J/(g*K)
0.2
-0,2
13
Identify − Makes Every User an Expert
As far as software-controlled automatic literature data from selected libraries, libraries, all data and exemplary
data handling is concerned, AutoEvalu- or to check whether a particular curve measurements from the NETZSCH
ation is not even the summit. NETZSCH belongs to a certain class. These classes “Thermal Properties of Polymers”
goes yet a step further and additionally may contain sets of data for various poster are provided. The Identify results
offers software which searches for types of the same polymer − e.g., are portrayed as hits sorted by degree
similar results stored in polymer several types of PE − but also curves, of similarity as a percent.
libraries, providing instantaneous such as ones which are classified as
interpretation of the measurement PASS or FAIL in terms of quality control. The plot below depicts the results of a
at hand. search for an unknown sample curve.
Both the libraries and the classes are The DSC curve for the best hit is shown
With the Identify software package, it boundless and editable; i.e., users can for direct comparison with the
is possible to carry out one-on-one extend them with experiments and unknown sample. The similarities are
comparisons with individual curves or knowledge of their own. As standard obvious: The unknown sample is PET.
DSC/(mW7mg)
exo
0,5
0,1
TION -0,5
I DE
NT -1,0
IF
IC 0 50 100 150 200 250
Temperature/°C
AT
IO
View of Identify results after only one click. The unknown curve is marked in green; the most similar
N
14
Identify...
PVAL PET 2 PET 1
64.48% 76.67% 95.93%
15
DSC 214 Polyma − Ideal for Quality Control of Polymers
16
Low-Temperature Performance
of Rubber DSC/(mW/mg)
0.50 exo
DSC measurements are important for Area: 4.85 J/g
58.4 °C
rubbers used in tires because their 0.45
Peak: 32.7 °C
Thermal Behavior of
Thermoplastic Polyurethane
DSC/(mW/mg)
182.3 °C
exo 206.9 °C
This plot shows a measurement on
Area: 10.19 J/g
TPU. During the 1st heating, the 0.50
17
DSC 214 Polyma − An Essential Aid for Process Optimization
In this example, two recycled polypropylenes were being used for injection
molding. Material A was completely crystallized after the molding process
whereas material B was still molten. To discover the reason for the differing
behavior, DSC measurements were performed.
exo
information. Besides the peaks at 1.2 Area: 87.11 J/g
Peak: 163.3 °C
165°C and 163°C, which are typical for
Material A
the melting of polypropylene, the blue 1.0 Material B
Area: 94.58 J/g
curve exhibits two additional peaks at Peak: 165.0 °C
18
Development of Process Parameters for Injection Molding
In the example, PBT with 30 wt% glass fibers was subjected to a temperature
program consisting of various cooling segments at cooling rates between 20 K/min
and 200 K/min.
200 K/min (black), the endothermic 100 120 140 160 180
Temperature/°C
200 220 240 260
19
DSC 214 Polyma − Sophisticated Measurement and Analysis
80 °C
The plot shows the degree of curing
60
for different isothermal temperatures.
A degree of curing of 95% is reached 70 °C
0 2 4 6 8
Time/min
20
Isothermal Crystallization of a
Semi-Crystalline Thermoplastic DSC/(mW/mg) Temp./°C
exo 300
6
Isothermal crystallization tests 296 °C
280
are often used to simulate the 4
Approx. 21 s
rapid cooling of finished polymer 260
parts during production 2
Temperature 237 °C
240
(e.g., injection molding).
0
220
DSC
The graph on the right depicts an -29.8 J/g
-2 200
isothermal crystallization experiment
on PA66 GF30 (containing 30 wt% 180
-4
glass fiber) using the DSC 214 Polyma
160
in combination with the IC70 intra-
-6
cooler. The low thermal mass of the 140
Arena furnace allows for a temper-
-8
ature interval of almost 60 K to be 120
21
Appendix
There are several relevant standards existing for application, evaluation and
interpretation of DSC data in the polymer field. The DSC 214 Polyma operates
based on all of them. A selection of standards can be found in the following table.
General
ISO 11357, Part 1 to 7 Plastics — Differential Scanning Calorimetry (DSC)
ASTM D3417 Heats of Fusion and Crystallization of Polymers by Thermal Analysis
ASTM D3418 Transition Temperatures and Enthalpy of Fusion and Crystallization by DSC
ASTM D4591 Temperatures and Heats of Transitions of Fluoropolymers by DSC
ASTM E793 Heats of Fusion and Crystallization by DSC
ASTM E794 Melting and Crystallization Temperatures by Thermal Analysis
ASTM E1356 Glass Transition Temperatures by DSC
Enthalpy of Fusion, Percent Crystallinity, and Melting Point of Ultra-High
ASTM F2625
Molecular Weight Polyethylene by DSC
DIN 50007 Differential Thermal Analysis (DTA): Basics (in German)
DIN 53545 Low-Temperature Performance of Rubbers (in German)
Heats and Temperatures of Melting and Crystallization by DSC of Electrical
EN 61074 (IEC 1074)
Insulation Materials
IEC 1006 Glass Transition Temperature of Electrical Insulation Materials
OIT
Polyethylene Plastics Pipe and Fittings Materials − Oxidative-Induction
ASTM D3350
Time
ASTM D3895 Polyolefins by DSC − Oxidative-Induction Time
Pipes, Fittings and Joints of Polyethylene-Type − PEM and PEH for Buried
DS 2131.2
Gas Pipelines
DIN EN 728 Polyolefins Pipes and Fittings − Oxidative-Induction Time
ISO TR 10837 Thermal Stability of Polyethylene for Use in Gas Pipes and Fittings
Resins/Curing
ISO 11409 Phenolic Resins − Heats and Temperatures of Reaction by DSC
Aircraft/Spacecraft: Testing of Thermosetting Resins with and without
DIN 65467
Reinforcement, DSC Method (in German)
22
Method
measuring cell
Software Proteus®
The software runs under the operating systems Windows XP,
Windows 7 and Windows 8.1.
23
The NETZSCH Group is a mid-sized, family-owned German company engaging in
the manufacture of machinery and instrumentation with worldwide production,
sales, and service branches.
The three Business Units – Analyzing & Testing, Grinding & Dispersing and
Pumps & Systems – provide tailored solutions for highest-level needs. Over
3,000 employees at 163 sales and production centers in 28 countries across
the globe guarantee that expert service is never far from our customers.
NGB · DSC 214 Polyma · EN · 3500 · 1013 · LH · Technical specifications are subject to change.
www.netzsch.com/n21467
NETZSCH-Gerätebau GmbH
Wittelsbacherstraße 42
95100 Selb
Germany
Tel.: +49 9287 881-0
Fax: +49 9287 881 505
at@netzsch.com