PRODUCT GUIDE / TA7000 Series - Haas

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Very small peak could be detected for analysis. Baseline ..... sample pan most suitable for the purpose of analysis. The
P R O D U C T G U I D E / TA 7 0 0 0 S e r i e s

Thermal Analyzer

TA 7000

S e r i DSC7000X

4

DSC7020

8

PDC-7 / PDC-7X

14

Sample pans and Sample sealer

15

S TA 7 0 0 0 S e r i e s

16

TMA7000 Series

22

DMA7100

28

Re a l Vi e w

34

TA 7 0 0 0 S o f t w a r e

38

System Network

42

Ti m e l i n e

43

e s

2 / 3

DSC

7000

Series

DSC7000X

High Sensitivity Differential Scanning Calorimeter

DSC7000X achieves unbeatable DSC sensitivity and repeatability with a superior new sensor and furnace. Hitachi High-Tech Science supplies the state of the art DSC for real experts.

New Sensor In this newly designed sensor multiple thermocouples guarantee high sensitivity, while the centric heat-flow method provides uniform and stable heat flow to sample and reference and therefore extremely stable baselines.

New Furnace Low heat capacity and three layer insulation design optimized by advanced computer modeling minimizes Influences of external condition and therefore avoid baseline fluctuation and improves in signal to noise ratio.

DSC7000X

DSC7000X with Auto Sampler

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DSC

7000

DSC7000X

Se r i e s

Fundamental Performance DSC7000X improves the reliability of data with its superior sensitivity, repeatability and expandability. The ability meet various applications such as high sensitivity measurement, direct sample observation and photochemical reactions as well as general DSC measurements makes DSC7000X the best choice for many DSC users.

0.50

200

30

400µW 50

0

Conventional

DSC (µW)

DSC (µW)

DSC (µW)

0.1µW 0.00

20µW

0

DSC (µW)

15

0.25

30µW 0

-200

-400

DSC7000X -15

-0.25

-600

-50 -30

-0.50

0

2

4 6 Time (min)

8

Twice the sensitivity compared to our conventional model. Very small peak could be detected for analysis.

10

-50

0

50

100

150

200

250

300

Baseline is highly stable which is four times superior to our conventional model. (Electrical Cooling Unit)

60

80

100

120

140

-800 140

160

180

200

220

Small amount of Polystyrene (PS)

Small amount of Carbamazepine

The above is a glass transition measurement of PS with the sample amount of only 0.105mg.

This also shows a high sensitivity performance of DSC7000X. The sample is only 0.03mg.

Temperature Control Performance Dramatically improved cooling capability enables accurate temperature control down to low temperatures. Both Auto LN2 Gas Cooling Unit and Electrical Cooling Unit can be connected at the same time, that eliminates troublesome cooling unit replacement.

100

500

100

600

400

50

50

400

300

0 -50

200

0

0

-50

200 100

Conventional

-100 DSC7000X

-150

Conventional -200

0

10

20

30 Time (min)

40

0

DSC7000X

50

60

0

50

100 Time (min)

150

200

-100

-100

0

10

20

30

40

50

Heating / Cooling cycle This shows the superior ability to control sample temperature at 10°C/min below -100°C using Auto LN2 Gas Cooling Unit.

Auto LN 2 Gas Cooling Unit

Stable sample temperature control at heating and cooling cycle at 20°C/min with Auto LN2 Gas Cooling Unit.

0

100

200 Time (min)

300

Heating / Cooling cycle Sample temperature curve at 10°C/min with Electrical Cooling Unit. Improved control ability keeps the linearity below -50°C.

Electrical Cooling Unit enables superior temperature control at heating / cooling cycle down to below -50°C (10°C/min) .

Electrical Cooling Unit

Temperature range: -150 to 725 Linear cooling rates below -100 at 10 /min 6 / 7

DSC

7000

Series

DSC7020

Differential Scanning Calorimeter

DSC7020 is a high-end versatile model with unique sensor that realizes high sensitivity and resolution performance. The superior basic performance together with the versatility makes DSC7020 ideal for various applications in both routine and research.

Unique Oval shaped Sensor The unique oval (ellipse) shaped sensor providing a shortest thermal path between sample and reference results in reduction of thermal resistance. This allows faster thermal response and improvement in resolution accordingly. Thermal path restricted by thermal filter between the main heat sink and small heat sink lowers the noise level and improves in sensitivity.

DSC7020

DSC7020 with Auto Sampler

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7000

DSC

DSC7020

Se r i e s

Improved Overall Performance Unique sensor design and improved ability in heater control gives drastically improved baseline and sensitivity performance. Lower noise level and baseline stability enable detection of week transitions with small amount of sample. Wide measurement range and use of Hitachi High-Tech Science pressure sample pans make DSC7020 best choice in a wide application range including safety evaluations.

0

0

DSC7020 Previous

-1

-20

-2 DSC (

DSC (

-40

-60

-3

-4

-80

-5

-100 60

80

100

120

140

-6 100

110

120

130

140

150

Small amount of Polystyrene (PS) / Sample weight: 0.18mg

High Resolution / Azoxyanisole resolution: 1.8

Above is a T g measurement result of PS. Improved sensitivity of DSC7020 allows detection of T g with only 0.18mg of sample.

This is a measurement of two closely occurring transitions of azoxyanisole. It shows improved resolution of DSC7020 over our previous model (DSC6200).

Full Line Options Cooling Unit A

Auto LN 2

B C

Gas Control Unit Flow Meter Gas Control

A

B

C

D

E

F

D

Unit*1

Mass Flow Control Unit*2

E F

Auto Sampler Unit UV Irradiation Unit Real View Sample Observation Unit *1 The electromagnetic valves and controller are built into the main unit. *2 The Mass Flow Control Unit is built into the main unit.

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DSC

7000

Se r i e s

DSC7000 Series Specifications

Model name Heat Flow Measurement Method Temperature Range Temperature Precision (Indium) DSC Measurement Range RMS noise / Sensitivity Calorimetric Repeatability (Indium) Scanning Rate Atmosphere Sample Pans* Gas Purge Control* Cooling Unit*

Cooling can Forced Air Cooling Unit Auto LN2 Gas Cooling Unit Electrical Cooling Unit

Auto Sampler Unit * Real View Sample Observation Unit* PDC-7 UV Irradiation Unit* *Optional

DSC7020

DSC7000X Heat flux

-170 to 725°C ±0.2°C ±350mW

-150 to 725°C ±0.1°C ±100mW

0.3J/g

0.1J/g 0.01 to 100°C/min Air, Inert gas flow

• Open pans (Aluminum, Platinum, Alumina) • Low-Pressure sealed pans (Aluminum, Chromated Aluminum) • High-Pressure sealed pans (Aluminum, Silver, Stainless-steel, Gold-plated stainless-steel) • Flow Meter • Gas Control Unit • Mass Flow Control Unit -170 to 725°C N/A Ambient to 725°C -150 to 725°C -70 to 420°C -80 to 500°C Available (max. 50samples, Mechanical arm transport, Quench cooling) Available Available

DSC7000X System

DSC7020 System

DSC Applications

20

10

0

100 Ganache

10

1st heating

5

-2

Lysozyme

50

Melting

2nd heating

-4 Ni : 0ppm Ni : 1000ppm Ni : 3000ppm Ni : 5000ppm

-6

50

100

150

200

250

300

0 Cocoa-rich Chocolate

-5

-10

-8

-20

68

70

72

74

76

DSC (µW)

Glass Transition

DSC (mW)

Crystallization

0

-10

DSC (mW)

DSC (mW)

Milk Chocolate

-40

0 Myoglobin

-50

-20

0

20

40

60

-100 50

60

70

80

90

100

Polyethylene terephthalate (PET)

Lead-free Solder

Chocolate

Protein

The above is a comparison of 1st and 2nd heating DSC curves of PET. In the 2nd heating (lower), Tg and cold crystallization peak are observed since the sample was converted to amorphous after rapid cooling.

This shows the DSC results for In35Bi2SnNi solder at different composition ratios. Unlike the eutectic melting peaks, there are differences in the solid-phase melting.

This is a comparison of DSC curves of three types of chocolates. The melting temperature varies according to cacao butter content.

This shows thermal denaturation measurements of 1% Lysozyme and Myoglobin solutions. DSC can be used to evaluate thermal stability of protein.

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PDC-7 / PDC-7X

Se r i e s

Option

UV Irradiation Unit

The photochemical reaction can be measured by both DSC7020 and DSC7000X with optional PDC UV Irradiation Unit. Reaction of photosensitive resin can be evaluated with different wavelengths and variable irradiation intensity which can be set precisely using digital UV intensity meter*. * Optional

Photochemical Reaction DSC System

Applications Wavelength dependency of Photoresist

Irradiation intensity dependency of UV curing adhesive 80

2.5 2.0

Irradiation Intensity mW/cm 2

Wavelength nm

365

60

405

500

1.5

DSC (mW)

7000

DSC (mW)

DSC

436 1.0

313 0.5

254

100

40

20 10 2

20

1

0

0 0

1

2 Time (min)

3

4

5

0

0.2

0.4 0.6 Time (min)

Specifications

Model name Temperature Range Light Source Light Guide Irradiation Wavelength Irradiation Range Wavelength-selective Filter* Irradiation Intensity Irradiation Intensity Adjustment Shutter Control *Optional

PDC-7 for DSC7020 PDC-7X for DSC7000X Ambient to 150°C Hg-Xe lamp (Quartz Type, 200W) Quartz Optical Fiber (D 5mm, L 1000mm) 240 to 550nm Sample / Reference 2 branching optical fibers system, Each D 8mm or more 254, 313, 365, 405, 436nm Maximum 500mW/cm2 or more 0 to 100%, in 0.1% increments Can be interlocked with temperature program

0.8

1.0

Sample Pans and Sample Sealer Open pans

Sealed pans Low-pressure

High-pressure

Gold plated stainless steel,

Chromated Aluminum,

Chromated Aluminum,

Aluminum plate for PDC, 7mm

Aluminum pan for PDC, 7 × H1mm

Aluminum for

Alumina, 5 × H5mm

Platinum, 5 × H5mm

Aluminum, 5 × H5mm

Copper, 5 × H2.5mm

Alumina, 5 × H2.5mm

Platinum, 5 × H2.5mm

Aluminum, 5 × H2.5mm

Various different types of sample pans in material, shape and volume are available for DSC measurement. Depending on property of sample and measurement condition it is important to use a sample pan most suitable for the purpose of analysis. There are roughly two types of sample pan, open type and hermetically sealed type. In hermetically sealed type, there are low-pressure type and high-pressure type. Sample sealer is used to crimp or hermetically seal sample pans before measurement. Crimping open type pan reduces internal temperature distribution for more accurate measurement. Sealing type pan prevents vaporization of water or volatilization of organic solvent. Electrical Sample Sealer can automatically crimp and seal sample pans only by pressing start button. It is especially useful in routine measurement or for auto sampler.

Sample Sealer

Electrical Sample Sealer

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S TA

7000

Series

STA7000

Series

Simultaneous Thermogravimetric Analyzer

STA7000 provides simultaneous measurement of both TG and DTA/DSC with a wide temperature range. The horizontal dual beam design ensures highly accurate and precise data enabling it to detect µg level weight change.

Holder

Furnace

Balance beam

Detectors

New Balance Control Technology – Horizontal Digital Dual Beam System – The newly-developed “Horizontal Digital Dual Beam System” guarantees excellent baseline stability and significantly low noise level ever seen in TG/DTA/DSC simultaneous analysis. Very small weight changes can be measured and analyzed without any time consuming baseline corrections. A/ D

A/ D

Fulcrum (Drive coil)

Horizontal digital differential system

STA7200

STA7200 with Auto Sampler

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S TA

7000

Se r i e s

Highly Precise Balance Control The highly sophisticated digital analysis of the weight and DTA difference of the dual beam system allows it to correct any environmental influences such as furnace, detector positions and thermal expansions of the beams.

60

Controlled Rate Thermal Analysis

(CRTA)

The CRTA is a measurement method which automatically controls heating rate according to the signal change of thermal analysis module. It is possible to separate the weight changes that occurs at very close temperature. The STA7000 series support the CRTA function as standard. The parameter can be chosen by the operator.

0

0

600

TG

CuSO4·5H 2O

0 500

-20

TG (%)

DTA

TG ( g)

DTA ( V)

0

CuSO4·3H 2O 300

-20

-60

200 -30

200

400

-100 800

600

-2H2O

CuSO4·H 2O -30

-H2O CuSO4

-40 -40

-40

-20

100

-80

-20

-10

400

-40

20

-2H2O

-10

80 g

TG (%)

40

0 0

30

60

90 120 Time (min)

150

0

50

100

150

200

250

Temperature (ºC)

Small amount of CaC 2O4

2

O

With only 0.13mg of Calcium Oxalate monohydrate, three distinct weight losses are precisely measured.

CRTA on CuSO 4·5H 2O

Comparison of CRTA and

Each step of multi-step dehydration are clearly distinguished, and the weight decrease rate at each step fits to the theoretical value.

standard method This shows CRTA ( ) more clearly isolate and detect each dehydration process than standard method ( ).

300

Optional Furnace tube

One Touch Designed Balance Beam

Vacuum Furnace Tube*1

Corrosive Gas Furnace Tube*1 *2

Vacuum Furnace Tube is another optional tube specially designed for measurement under vacuum or reduced pressure. 1.3Pa can be achieved with this optional tube and external pumping system.

Corrosive Gas Furnace Tube can be used for measurement under special atmosphere such as corrosive gases. It enables such measurement without damage of the balance mechanism.

The one touch type balance beam design allows users to replace the beams easily by themselves. Light weight balance beam enables STA7000 series to provide highest sensitivity and stability performance.

*1 Optional *2 There are limitations on the types of corrosive gases that can be used with corrosive gas furnace tube.

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S TA

7000

Se r i e s

STA7000 Series Specifications

Model name Balance System Temperature Range Scanning Rate TG Measurement Range TG RMS noise / Sensitivity DTA Measurement Range DTA RMS noise / Sensitivity Maximum Sample Weight Atmosphere Purge Gas Flow Rate Gas Purge Control* Sample Pans* Cooling Unit Auto Sampler Unit * Real View Sample Observation Unit* *Optional

STA7200

STA7200RV Horizontal Differential Type Ambient to 1000°C

Ambient to 1100°C 0.01 to 150°C/min

N/A

STA7300 Ambient to 1500°C 0.01 to 100°C/min

±400mg 0.1 g / 0.2 g ±1000 V 0.03 V / 0.06 V 200mg • Air, Inert gas flow • Vacuum* (to 1.3Pa) 0 to 1000mℓ/min • Flow Meter • Gas Control Unit • Mass Flow Control Unit • Open pans (Aluminum, Platinum, Alumina) • Auto Fan Cooling Unit • Forced Air Cooling Unit Available (max. 50samples, mechanical arm transport) Available

STA7300 System

N/A

STA7200RV + RV-3TG System

STA Applications 10

0 155.9

PC

-40

30.9 J/g

DSC

-5

-60

251.6

-10

400

500

800

10

200

300

400

500

600

-100

DSC

0

-150 m/z 44

-100

5

-200

m/z 28

MS 0

-100 100

-50

-86.0%

-15 200

15

-80 436.3

0

0

100

DTA (µV)

0

29.0J/g

MS Intensity

PET

-80 -100

20

TG (%)

HDPE -60

-20 76.4

PI

PS

-40

519

TG

5

PTFE

PMMA

DSC (mW)

TG (%)

-20

200

25

TG

TG (%)

0

-200

-250 200

700

Thermal decomposition of Polymers

TG/DSC measurement of

This is a comparison of TG results of various polymers. It shows that thermal decomposition behavior differs by polymer type.

Polyethylene terephthalate (PET)

8.0E+06

DSC result shows the calorimetric analysis for crystallization and melting and TG result shows weight change by thermal decomposition.

6.0E+06

400

44

600

m/z 44 CO 2

4.0E+06 2.0E+06

28

m/z 28 CO

12

0.0E+00 m/z 10

20

30

40

50

60

70

80

TG-MS analysis of Fullerene C70 Weight loss was detected by TG at identified by MS as CO and CO2.

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TMA 7000

Series

TMA7000 S e r i e s

Thermomechanical Analyzer

TMA7000 series have great flexibility with various measurement modes to meet many different applications. With the capability of stress-strain control, TMA7000 series provide analysis of dynamic characteristic as well as static and dynamic viscoelastic measurement.

Expansion

Penetration

Cone

Designed to meet all Application needs

Tension

Bending

Volume Expansion

Metal Tension

Alumina Expansion

Wide dynamic ranges: Measurement range ±5 mm, Load range ±5.8 N, Maximum sample size; D 10 × L 25mm. Stress-Strain, Creep / Recovery, Stress-Relaxation, and DMA measurements increase the value of use above the conventional TMA measurements such as thermal expansion, glass transition and softening. The complete range of measurement probes and cooling units covers all application needs.

TMA7000 Series

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TMA 7000

Se r i e s

Excellent Heating and Cooling Performance

Wealth of Cooling System LN 2 Dewar Vessel

A

Auto Fan Cooling Unit*

B

Auto LN 2 Gas Cooling Unit*

C

Electrical Cooling Unit*

D

TMA7000 series provide superior temperature control performance in wide temperature range. High sensitivity measurement can be carried out even at low temperatures.

0.0 A

200

B

TMA

TG (%)

-0.5

100 -45.1ºC -44.9ºC

-1.0

-45.2ºC -45.1ºC

0 -1.5 -100

Temperature -2.0 0

C

*Optional

D

20

40

60 80 Time (min)

100

120

In this TMA measurement, natural rubber was cooled and heated repeatedly using Auto LN2 Gas Cooling Unit. Its excellent temperature control performance can be seen from the data reproducibility in glass transition measurement.

Stress-Strain Capabilities 300

The TMA7000 series has stress strain measurement and analysis capability. Stress-Strain characteristic, Creep/Recovery, Stress Relaxation can be measured, and furthermore, applying sinusoidal force to samples the dynamic viscoelastic behavior can be characterized.

5

200

0

100

-5

Load

Load

TMA 0

100

-15 150

1010

1010

0.600

0.6

12 10

0.4 109

0.400

E” 109

108

0.200

108

-100

8 0.2

6 1.55x10-5J

1.77x109Pa

4 0.0

tan

107

Stress (N/cm2)

50

tan

0

E (Pa)

-50

E” (Pa)

-200 -100

-10

53.0ºC

2

-50

0 50 Temperature (ºC)

100

0.000 150

0 -4.8

-0.2

-4.6

-4.4 Strain (%)

-4.2

4.0

-50

0

50

100

150

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TMA 7000

Se r i e s

TMA7000 Series Specifications Model name Temperature Range Scanning Rate Sample Tube

Probe

Probe Supporting Method TMA Measurement Range RMS noise / Sensitivity Load Range / Resolution Maximum Sample Dimensions Sample Length Measurement Atmosphere

Stress Control Mode Strain Control Mode Gas Purge Control* LN2 Dewar Vessel Auto Fan Cooling Unit* Cooling Unit Auto LN2 Gas Cooling Unit* Electrical Cooling Unit* *Optional

TMA7100 -170 to 600°C

TMA7300 Ambient to 1500°C

0.01 to 100°C/min • Quartz • Metal* • Alumina • Quartz* • Quartz Expansion Probe • Alumina Expansion Probe • Quartz Penetration Probe* • Quartz Expansion Probe* (to 1000°C) • Quartz Cone Probe* • Quartz Penetration Probe* (to 1000°C) • Quartz Tension Probe* • Quartz Cone Probe* (to 1000°C) • Quartz Bending Probe* (to 500°C) • Quartz Tension Probe* (to 600°C) • Volume Expansion Accessory* (Ambient to 200°C) • Quartz Bending Probe* (to 500°C) • Metal Tension Probe* Cantilever ±5mm ±5.8N / 9.8 N ±1.47N / 9.8 N Expansion, Penetration: D 10 × L 25mm Expansion: D 10 × L 25mm Tension: W 5 × T 1 × L 25mm Automated Measurement • Air, Inert gas flow • Vacuum* (to 13Pa) • Air, Inert gas flow • Swelling* (to 80°C) • Vacuum* (to 13Pa) • Humidity control* (to 90°C, 90%RH) • Constant Loading: ±5.8N • Constant Rate Loading: 9.8 × 10-2 to 9.8 × 106mN/min • Sinusoidal Loading: 0.001 to 1Hz • Combination: maximum 40 steps • • Constant Rate Strain Control: 0.01 to 106 m/min • Sinusoidal Strain Control: 0.001 to 1Hz • Combination: maximum 40 steps • Flow Meter • Gas Control Unit • Mass Flow Control Unit -170 to 600°C N/A Ambient to 600°C Ambient to 1500°C -150 to 600°C N/A -60 to 450°C N/A

TMA7100 System

TMA Applications

1.5

200

400

20

-69ºC 187.3ºC

15

0.5

300

TD

TMA (%)

6.40x10-5 (1/º

TMA (µm)

1.0 TMA (%

161.4ºC

-200

74.8ºC

PE

PP

10

MD

5

Nylon

Stress (kg/cm2)

114.8ºC

0

200

-35ºC -12ºC

100

-400

5ºC 25ºC 47ºC 62ºC

0

2.55x10-4 (1/º

0.0 0

20

40

60

80

100

120

-600

0

-5 0

50

100

150

200

250

20

40

60

80

100

120

0

5

10 Strain (%)

15

Thermal Expansion of

Penetration on Polymer film

Anisotropy of Polyethylene (PE) film

Stress-Strain characteristic of

Polyvinyl chloride (PVC)

Comparison of softening temperatures between different polymer films, Polyethylene, Polypropylene and Nylon evaluated by penetration measurement.

In above measurements of PE film, tension force is applied in machine direction (MD) and the transverse direction (TD).

Polyethylene (PE) film

CTE (coefficient of thermal expansion) changes at the glass transition temperature. CTE after T g is approximately 4 times larger.

20

The measurements are carried out on PE film with strain control mode at different temperatures.

14 / 27 26 15

DMA 7100

DMA7100

Dynamic Mechanical Analyzer

With its advanced overall performance and user-friendly design, DMA7100 is ideal for routine and research use. Navigation guide in the software and the simple sample clamping design allows for operation without difficulty.

Tension

Tension Spring Chuck

Variety of Deformation Modes

Dual-Cantilever Bending

3-Point Bending

Compression

Shear

Film-Shear

As standard the DMA7100 comes with the tension attachment. To be able to measure samples with different characteristics a variety of optional attachments are available. This ranges from Dual and Single Cantilever Bending, 3-Point Bending with different active lengths, Shear and Film-Shear, to Tension and Compression. This allows characterization of all sample shapes as well a single fiber as stiff bulk samples.

DMA7100

28 / 29

DMA 7100

Synthetic Oscillation Mode

In this mode, measurement is proceeded with synthesized waveform from five different frequencies. This allows one to apply multiple frequencies on samples which undergo drastic softening in a very narrow temperature range.

Simple Measurement Wizard

Any users who are unfamiliar with DMA can operate DMA7100 with the Simple Measurement Wizard. It guides you with easy-to-follow navigation in every step from condition setting to measurement.

Lissajous Monitor DMA7100 is equipped with Lissajous monitor for observing the relationship between stress and strain of the sample under measurement. With Lissajous monitor, the deformation of the sample can be verified in real time and also after measurement at every measurement point, thus reliability of data acquisition improves.

14 / 31 30 15

DMA 7100

DMA7100 Specifications Model name Deformation Mode Measurement Range (1Hz) Measurement Mode Frequency Force Range Elasticity Reproducibility tan Measurement Range tan Resolution / RMS noise Temperature Range Scanning Rate Temperature Program Mode Atmosphere Gas Purge Control Forced Air Cooling Unit Cooling Unit* Auto LN2 Gas Cooling Unit Real View Sample Observation Unit* *Optional

DMA7100 Dual-Cantilever 3-Point Tension Shear Film-Shear Compression Bending Bending 105 to 1012Pa 105 to 1012Pa 106.5 to 1013.5Pa 103 to 109Pa 104 to 1010Pa 105 to 109Pa • Dynamic Measurements: Sinusoidal wave oscillation mode / Synthesis wave oscillation mode • Static Measurements: Program stress control / Program strain control • Sinusoidal wave oscillation: 0.01 to 200Hz, maximum 20 frequency • Synthesis wave oscillation: 5 frequency • Dynamic Force: ±10N • Static Force: ±10N • Tension (Aluminum): 69.1Gpa ± 2Gpa (1Hz) • Bending (Steel): 192GPa ± 2Gpa (1Hz) 0.0012 to 9.9999 within 0.000001 / within 0.0001 -150 to 600°C 0.01 to 20°C/min • Ramp Mode (maximum 100 steps) • Step Mode (minimum temperature step 0.01°C) • Air, Inert gas flow • Swelling* (to 80°C) 300mℓ/min (A Gas Flow Controller is built in to the main unit as standard.) Ambient to 600°C -150 to 600°C Available DMA7100 System

DMA Applications

1010

3.000

1010

108

104

E (Pa)

2.500 E”

2.000

106

By performing the simultaneous measurement of temperature dispersion and frequency dispersion measurement, relaxation phenomena such as glass transition, crystal relaxation, and said chain relaxation, etc., can be observed. It enables to obtain the information of molecular structure and molecular motion of polymer.

1.500 1.000

104

0.500 tan 0.000 200

Polymethylmethacrylate (PMMA) Simultaneous measurement result of temperature dispersion and frequency dispersion for PMMA.

1012

1010

3.500

109

3.000

115.3ºC

3.000

1010

108

106

104

E”

2.500

117.3ºC

108

E”

2.000

106 131.8ºC

1.500 1.000

104

2.000

108

tan

100 150 Temperature (ºC)

E , E” (Pa)

50

tan

102

E (Pa)

102

E” (Pa)

E” (Pa)

108

106

3.500

tan

1012

1.000

107 tan

0.500 102

102

tan 50

100 150 Temperature (ºC)

0.000 200

106 10-3

10-2

10-1

100

101

102

0.000 103

Frequency (Hz)

Temperature Dispersion Data

Frequency Dispersion Data

Viscoelastic property change is analyzed with respect to temperature.

Frequency dependency of viscoelastic property at different temperature is analyzed.

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TA 7 0 0 0

Re a l

Real View

Vi e w

Sample Observation System

Real View Sample Observation System allows visual inspection of the samples during measurement and analysis of images after measurement. Analysis of sample property change from visual aspect such as color and shape is now available in addition to conventional thermal analysis.

STA7200RV

DSC7000X

View Port

Sensor Quartz window lid

Sample Holder

Quartz furnace tube

Real View DSC System

Real View STA System

Real View DMA System

34 / 35

TA

7000

Re a l

Vi ew

Visualizing the Imaginary World There are two different ways to display images obtained in Real View measurement. Images, DSC, TG, and DMA data are all linked and relation between state of sample and temperature can be observed clearly.

Thumbnail View By clicking a point on data curve, the corresponding image and some sequential images around the selected point will be displayed.

Slide Show This mode plays a series of images to create a movie. Subtle changes in color, shape or morphology over time can be visually analyzed.

Length Measurement Function The length of the sample before and after the shape change can be measured by Length Measurement Function.

0

10 TG

-20

Digital Zoom Function

Tg

DSC

-40 -10

-60 -20

TG (%)

DSC (mW)

0

-80 -100

-30 100

200

300

400

500

Real View TG Measurement of Plastic Optical Fiber

Digital Zoom Function may provide more information by zooming a part of an image. 5 different magnifications with maximum 5.7 times are available.

This is a measurement of Plastic optical fiber that is made of PMMA as the core material and Fluorine resin as the clad. Shape change caused by residual strain around the glass transition temperature, and the process of thermal decomposition from 300 to 500°C is clearly visualized.

36 / 37

TA

7000

Thermal Analysis Software

Software Package Innovative Technology-Multi Module Analysis

Simplify Your Analysis

Perform simultaneous analysis of different technologies in one diagram.

TA7000 Software is designed to work in Windows OS environment. The analysis results are exported to Word and Excel with one click. The user is free to use other commercial software for further calculation and display.

Different measurement results can be analyzed in same screen. Easy to compare the analysis results by different methods.

Customized Performance · Selection of all operation icons to your own needs. · Arrangement of the layout according the measurement conditions.

Advanced Software Specific Heat Calculation

Purity Analysis

Modulated DSC Conversion

Kinetics Analysis

Calculate the specific heat capacity (Cp) from DSC measurement data.

Determine the purity of a sample by evaluating its melting peak measured by DSC.

Converts the temperature modulated DSC data to the Total Heat Flow, the Reversing, and the Nonreversing Component.

Calculate the activation energy ( a) of chemical reactions from TG and DSC measurement data.

ISO 11357-4

ASTM E1269

JIS K 7123

ASTM E928

ISO 11358-2

ASTM E1641

ASTM E2602

4

DSC (mW)

99.3%

100%

-5

150

15

20

-10 120

-50

-4 130

125

135

140

134.5

Purity: Melt. Point: Correct Delta H: Correct %: Standard Dev.: Molecular Weight:

134.0 Temperature (ºC)

2.5

2.0

1.5

133.5

99.28 % 134.3 °C 35.33 kJ/mol 3.38 % 0.001 179.22

133.0

80

100

Temperature (ºC)

120

140

0.00

10

15

20

25

2.00

4.00

6.00 1/F

-60

-80

0

-100 250

30

300

8.00

10.00

400

350

4

R.F. % 20 40 60 80

1.50 2

Nonreversing

0 Total Heat Flow

-4

450

550

500

Temperature (ºC)

Delta E kJ/mol 160.578 163.188 169.343 172.261

Life Time kday 8.6E+01 2.1E+02 6.6E+02 1.4E+03

1.00

0.50

-2

132.0

60

5

-40

Time (min)

132.5

1.0

40

0

Temperature (ºC)

DSC (mW)

10 Time (min)

50

Temperature

3.0

20

-20

100

0

Sample

0.5

200

0

-2

-8 -10

Cp (J/g·deg)

DSC

ogB (ºC/min)

0 DSC (mW)

50

Standard

2 Temperature (ºC)

DSC (mW)

100

-4

5

0

TG (%)

150

-2

0

250

Temperature (ºC)

Empty pan

-6

4 98%

0

-12

5

200

2

Reversing

50

100

150

Temperature (ºC)

200

0.00 1.200

1.300

1.400

1.500

1.600

1.700

1000/T (1/K)

38 / 39

7000

TA

T h e r m al Analysis

Software

Viscoelasticity Conversion

Master Curve

Activation Energy

Composition Calculation

Convert the TMA measurement data to dynamic mechanical analysis data and analyze the viscoelasticity properties.

Generate the master curves using the Time-Temperature Superposition Principle for the estimation of mechanical properties at very high or very low frequencies.

Calculate the apparent activation energy from temperature and frequency dispersion measurement results.

Calculate the viscoelastic properties of a coating layer from the measurement results of a sample ( ) and substrate ( ).

300

1010

5

2.500

101

1010 1010

Load 109

1.000

108

100

E”

tan

108

109

E (Pa)

108

E” (Pa)

1.500

E (Pa)

-5

Load

100

2.000

109

0

tan

200

10-1

TMA

50

100

1010

-15 150

106

0.200

108

106 tan

10

108

-100

120

140 Temperature (ºC)

160

106

tan

180

Delta E 394.468 kJ/mol

102

10-2

-100

0 100 Temperature (ºC)

200

1011

10 1 10 11

E’

2.000

1.000

E”

101 1010

100

E” 109

10-1

10 0

10 10

10 -1

10 9

0.100

10-2

tan 107

0.000 100

100

tan

E , E” (Pa)

tan

E (Pa)

E” (Pa)

0.300

109

0.1 1 Frequency (Hz)

3.000

108

E”

0.01

MasterCurve 115.0ºCParameter Shift Mode: WLF Tg = 115.00ºC Tr = 115.00ºC C1 = 11.00 C2 = 42.00

0.400 109

106

0.500

1010

0.500

107

tan

0

107

(Pa)

1010

-50

107

E” (Pa)

-200 -100

-10

Frequency (Hz)

0

-50

0 50 Temperature (ºC)

100

0.000

104

10-8

10-6

10-2 10-4 Frequency (Hz)

100

102

0.000

108

2.200

2.300

2.400

2.500

1000/T (1/K)

2.600

2.700

tan 10 8

10 -2

-100

0 100 Temperature (ºC)

200

Auto Analysis The Waveform Separation Software includes following three functions. The application to the conversion to high-resolution data or an evaluation of heating rate dependence is possible.

Peak Separation for DSC and

Profile Separation for TG and

Heating Rate Conversion

DTA peak

TMA curve

Simulation for DSC and TG curve

10

0

0

The analysis software starts up automatically after end of a measurement and executes the data analysis, the printout of data, and save the analysis result. In the combination with the Auto Sampler Unit, the whole process can be automated from the measurements to the printout of the analysis results.

10ºC/min 5 -20

0

External Data Import

TG (%)

TG (%)

DSC (mW)

-10

-20

-40

-5

-10

0

50

100

150

-30

200

0

50

100

150

-60

200

100

Temperature (ºC)

Temperature (ºC)

10

200

300

400

Temperature (ºC)

0

21 CFR Part11

0

5 -20 0.1ºC/min

TG (%)

TG (%)

DSC (mW)

0

-20

1ºC/min

-40

-5

-10

0

50

100 Temperature (ºC)

150

200

-30

0

50

100 Temperature (ºC)

150

200

-60

100

200

300

*Optional

It supports requirements, access control, electronic signature, and audit trail, in the 21 CFR Part11 by FDA of USA.

10ºC/min -10

External data is imported in measurement result by text data. It is available for analysis by TA7000 software as well as thermal analysis data.

400

Temperature (ºC)

40 / 41

TA

7000

Sy st e m

N etwork

TA7000 System Network The TA7000 series, with extensive range of instruments for thermal analysis, delivers complete solutions for thermal property characterization. Multiple instruments can be controlled by one PC station that is space and cost saving. Data analysis after/during the measurement can be performed from your PC. The measurement status can be notified by e-mail or pop-up message on your mobile phone. DSC7000X STA7000 Series

LAN DSC7020

Wireless LAN

Display message

TA7000 Software Server

DMA7100

TMA7000 Series

Off-line data analysis

Timeline

Timeline of HITACHI Thermal Analysis Products

Highly Trusted Brand with remarkable achievements Since the first model in 1974, Hitachi High-Tech Science has been a pioneer in developing and manufacturing thermal analysis instruments. With over 40 years of experience and having operational bases worldwide, we are confident in providing state of the art instruments and solution, always as ever.

1970

Adiabatic Scanning Calorimeter SSC510 Scanning Conduction Calorimeter SSC540 Reaction Heat Calorimeter / Vaporization Heat Calorimeter SSC630 High Sensitive Scanning Conduction Calorimeter SSC544 Photochemical Reaction Calorimeter SSC550 SSC560 Series

SDM5600 Series

TA7000 Series

DMS120, DMS210, DES100

DSC7000X, DSC7020

SSC5100 Series

STA7200, STA7200RV

DSC22, TG/DTA22

STA7300, TMA7100 TMA7300, DMA7100

560U, 560S(DSC), 560G, 560GH 560GX(TG/DTA), 560M(TMA)

TG/DTA6300, TG/DTA6200R TG/DTA6300R, TMA/SS6100 TMA/SS6200, TMA/SS6300, DMS6100

1980

1990

EXSTAR6000 Series DSC6100, DSC6200, DSC6300 DSC6200R, TG/DTA6200

2000

2010

SSC580 Series

SDM5500 Series

EXSTAR7000 Series

DSC10, DSC20, DTA30 TG/DTA20, TG/DTA30, TG20, TG30 TMA10, TMA20, TMA30, TMA/SS10

DMS100, DMS200

X-DSC7000, DSC7020 TG/DTA7200, TG/DTA7300 TMA/SS7100, TMA/SS7300

SSC5000 Series

PDC121, TG/DTA220, TG/DTA320 RTG220, TMA120, TMA320 TMA/SS120, TMA/SS150, TMA/SS350

DSC100, DSC200, DSC300, PDC150 TG/DTA200, TG/DTA300 TMA100, TMA300, TMA/SS100

1974 - Adiabatic Scanning Calorimeter SSC510

SSC5200 Series DSC120, DSC220, DSC320, RDC220

1982 - SSC580 Series

1986 - SSC5000 Series

2014

DMS7100

1995 - EXSTAR6000 Series

2007 - EXSTAR7000 Series

2014 -TA7000 Series 42 / 43

Science Ring

This logo symbolizes Scientific and Analytical instruments of Hitachi High-Tech Group. It is composed with an “S”, standing for "Science", our technology core competency, and with a ring that represents close connection we make with our customers. This “Science Ring” shows how we are committed to create new values by strengthening ties between Science and Society.

The above logo is a registered trademark of Hitachi High-Technologies in the United States and other countries.

Note: To ensure safe operation, follow the instruction manual when using the instrument. / System specifications are subject to change without notice. / The PC monitor shows composite images. / “Windows”, “Word” and “Excel” are registered trademarks or trademarks of Microsoft Corporation in the United States and other countries.

Head Office Sales Division 24-14, Nishi-Shimbashi 1-chome, Minato-ku, Tokyo 105-0003, Japan

http://www.hitachi -hightech.com/hhs/

Hitachi Instruments (Shanghai)Co., Ltd. Hitachi High Technologies America, Inc. Hitachi High-Technologies Europe GmbH [Mannheim office]

http://www.hitachi-hightech.com/hig http://www.hitachi-hightech.com/us/ http://www.hitachi-hightech.com/eu/

HAAS. 60175 Poznań, ul. Bratkowa 9, tel. +48 61 622 95 80, mob. +48 501 450 410, www.haas.com.pl, [email protected]

2016-HHS-TA01/2016.2