Nova Geração de Instrumentos de Análise Térmica

Transcription

1 Nova Geração de Instrumentos de Análise Térmica IV ENCONTRO REGIONAL DOS USUÁRIOS DE TÉCNICAS TERMOANALÍTICAS Jul/2009

2

3 Thermal Analysis Technology

4 EXSTAR SERIES Thermal Analyzer DSC7020 (Differential Scanning Calorimeter)

5 DSC Applications Physical Change Melting Crystallization Glass Transition Evaporation Sublimation Magnetic Transition Specific Heat Capacity Information Melting point (Tm) Melting enthalpy (Delta Hm) Crystallization temperature (Tc) Crystallization enthalpy (Delta Hc) Glass transition temperature (Tg) Heat capacity change at Tg (Delta Cp) Temperature Curie Point Specific Heat Capacity (Cp)

6 DSC Applications Chemical Reaction Cure Reaction Oxidation Reaction Decomposition Chemisorption Desorption Others Micelle Formation Thermal Denaturation Gelatinization Information Reaction temperature Reaction enthalpy Reaction temperature Reaction enthalpy Reaction temperature Reaction enthalpy Chemisorption / desorption temperature Chemisorption / desorption energy Information Krafft point Energy Thermal denaturation temperature Thermal denaturation enthalpy Gelation point

7 Heat Flux DSC (Differential Scanning Calorimeter)

8 DSC 7020 OVAL SENSOR Reference Pan Oval Sensor Plate Sample Pan Heater Sub Heat Sink Oval Sensor Plate Main Heat Sink Oval DSC Diagram Heat Filter Main Heat Sink Lead Wire Oval DSC Cross Section High Resolution (Quick responsibility) Low thermal resistance by 2nd dimension thermo flow The shortest heat flow between sample and reference Protect the sensitivity down (by reducing noise lever) Heat sink substrate used as sensor holder also Filter stored inside sensor in order to cut the noise.

9 DSC7020 Module DSC Type Temperature Range Temperature Reproducibility Dynamic Range RMS Noise/ Sensitivity Temperature Rate Environment Sample Pan Gas Purge Control Cooling Unit Auto-sampler Temperature Range DSC7200 Heat Flux -160~725 ±0.1 ±350mW 0.1μW/0.2μW 0.01~100 /min Air, Inert Gas Open (Al) 100μl Hermetic (Al Alozine) Sealed (Al Ag SUS SUS ) l Mass Flow (Optional) Gas Controller (Optional) Automatic LN2, Electronic Cooling system, Air Cooling (Optional) 50 Positions, Mechanic Arm( Optional) 15μ Automatic LN2 cooling unit:-140~ 725 Electronic Cooling system :-75~550 Air Cooling :Ambient~725

10 DSC μw Performance Criteria 1.Stable baseline 2.High sensitivity High resolution Reproducibility C/min Temp. Baseline performance is quantified by determining the amount of curvature and drift over a specified temperature range

11 DSC μw Performance Criteria Stable baseline 2.High sensitivity 3. High resolution DSC6220 DSC Reproducibility C/min Temp. Baseline performance is quantified by determining the amount of curvature and drift over a specified temperature range

12 DSC/ uw DSC / uw Performance Criteria Indium:0.003mg, 1C/min 1.Stable baseline High sensitivity 3. High resolution 4. Reproducibility Temp / 86.3 C Polystyrene:0.18mg, 10C/min Temp / DSC sensitivity is a function of the signal to noise ratio of the heat flow signal, as well as baseline quality for step transitions

13 Performance Criteria 1.Stable baseline 2.High sensitivity 3.High resolution 4. Reproducibility Resolution=1.8 Sample: Azoxyanisole DSC:DSC7020 Sample weight:5mg Scan Rate:20 C/min

14 DSC mw Performance Criteria 1.Stable baseline 2.High sensitivity 3.High resolution 4.Reproducibility In, n=5 10mg, 10C/min Temp.

15 DSC mw Indium H/W Ratio Test Condition 2.00 Sample Material Sample Mass Indium (> 99.5% purity) 1.0±0.1 mg , 28.6J/g Pan Type Purge Gas Standard aluminum (note any exception) Nitrogen (no exceptions) Flow Rate 20 ml/min (or manufacturer s recommendation) Data Collection Rate < 10 pts./s Thermal Method 120 to C/min (cycled if desired) Indium:1mg, 10C/min H/W= Temp

16 D SC / mw D SC / mw SUPER HIGH SENSITIVITY Lead Free solder : 10mg 10C/min In35Bi2Sn In35Bi2Sn0.1Ni In35Bi2Sn0.3Ni In35Bi2Sn0.5Ni Tem p / Tem p /

17 D SC / uw SUPER HIGH SENSITIVITY D SC / uw Two pieces of copy paper (5mm X 5mm) Two pieces of copy paper ( 5mm X 5mm ) 10C/min measurement result of the toner Tem p / toner:12mg 10C/min Tem p /

18 Application of Highway TA Research & Development Application ー Utilizado para DSC e TGA. ー Simulação de análises de dados na qual atingimos temperaturas extremamente altas (ex. 10,000 /min) ou extremamente baixas (ex. 0,001 /min). Diminuição do tempo de análise para controle de qualidade em até 1/10 do tempo.

19 Principle of Highway TA l o g B Heating Rate of measurement High Heating Rate data Slope ΔE Low Heating Rate data 1/T Highway TA Conversion Principle T : Temp. B : Heating Rate

20 Peak Separation Synthetic Peak Measured Data Separated Peak

21 Highway TA 0.00 Poliamida 5ºC/min 10ºC/min ºC/min 20ºC/min 25ºC/min Temp Cel

22 EXTENSIBILITY Full range Cooling system Electronic Cooling System, Automatic LN2 cooling system Robust Auto-sampler

23 Sample Sealer & Sample Pan Easy Operation High Reproducibility Sample Pan 1-7 Sealed Type 8-15 Open Type Hermetic Type Alumina Pan Al Alodine Processed 15ml Al Auto-sampler Alumina Pan

24 Thanks for your Attention Sérgio Azuma Cirlene Fourquet IV ENCONTRO REGIONAL DOS USUÁRIOS DE TÉCNICAS TERMOANALÍTICAS Jul/2009