A Short Reviews of Thermal Techniques

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3 A Short Reviews of Thermal Techniques DSC TGA ( ).. [ ] [ ] Heat Flux Torque converter Null Type Balance. Power Compensation [ ] [ ] / (Tg) / (Tm) ( )/ Oxidative Induction Time Oxidative Induction Time / Polymorphism / Curie Point Fingerprint etc. etc.

4 TMA. (Non-Oscillating mode) [ ] Magnetic force motor Drive force motor [ ] Static Modulus/Young s Modulus (CTE) Dilatometry Tg, Tm Extension Test etc. DPA SDTA STMA DEA TG-MS TG-IR ADSC(MDSC) Maxres TGA TTS DM(T)A. [ ] Fixed frequency Resonant frequency [ ] Dymamic moded modulus(storage, loss M) Tangent delta Tg, Tm Low energy transition / Long term Mechanical property Miscibility study / etc.

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8 Power Compensation DSC Quantitative DTA Measures dh directly Uses platinum resistance thermometers Derives dh Uses thermocouples

9 Temperature or Time

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18 Effect of Sample Size on Sensitivity and Resolution 100 Indium Indium Indium mg mg mg Peak = Heat Flow (mw) Peak from: to: Onset = J/g = Peak from: to: Onset = J/g = Peak from: to: Onset = J/g = Peak = Peak = o Temperature ( C)

19 Heat Flow (mw) Curve 1: DSC File info: hdpe2 Thu Jul 12 14:18: Sample Weight: mg High Density 10C/min X X Peak Area mj H J/g Height mw Onset C C C C TEMP1: 15.0 C TIME1: 0.0 min RATE1: 10.0 C/min TEMP2: C Temperature ( C) Application Laboratory PERKIN-ELMER 7 Series Thermal Analysis System Mon Aug 22 13:16:

20 Heat Flow (mw) Curve 1: DSC File info: polye Mon Jul 22 12:23: Sample Weight: mg POLYESTER INITIAL HEATING # 1 POLYESTER INITIAL HEATING:polye Heat Flow (mw) # 2 POLYESTER AFTER QUENCHING FROM THE MELT Heat Flow (mw) TEMP1: 40.0 C TIME1: 0.0 min RATE1: 40.0 C/min TEMP2: C Temperature ( C) PERKIN-ELMER 7 Series Thermal Analysis System Mon Aug 22 13:40:

21 Heat Flow (mw) Analysis of Low Melting Wax Curve 1: DSC File info: dtc02 Mon Feb 20 16:12: Sample Weight: mg Dotriacontane 2 C/min Peak H J/g C 45.0 Peak H J/g C Onset C Onset C TEMP1: 50.0 C TIME1: 0.0 min RATE1: 2.0 C/min TEMP2: 74.0 C Temperature ( C) B.Cassel PERKIN-ELMER 7 Series Thermal Analysis System Mon Aug 22 13:47:

22 CALORIMETRY CONSIDERATIONS SAMPLING VARIABLES SAMPLE SIZE SAMPLE GEOMETRY SAMPLE PANS SAMPLE CONDITIONING

23 CALORIMETRY CONSIDERATIONS INSTRUMENTAL/TEST VARIABLES SCAN RATE PURGE GAS CALIBRATION COOLANT

24 Heat Flow (mw) CONSTANT CALORIMETRY REGARDLESS OF SAMPLE SIZE. Curve 1: DSC File info: indium004 Tue Feb 14 16:30: Sample Weight: mg Indium (4.998mg.) Peak H J/g Indium mg. C Peak Indium mg. H J/g C Indium mg. Peak H J/g C Indium Onset CIndium mg. mg. Indium mg. Onset C Indium mg. Onset C CALORIMETRIC TEST TEMP1: C TIME1: 0.0 min RATE1: 10.0 C/min TEMP2: C Temperature ( C) Tech.Support Lab PERKIN-ELMER 7 Series Thermal Analysis System Wed Feb 15 12:18:

25 SAMPLING VARIABLES SAMPLE GEOMETRY GEOMETRY AFFECTS PEAK HEIGHT GEOMETRY AFFECTS PEAK WIDTH GEOMETRY AFFECTS PEAK POSITION GEOMETRY DOES NOT AFFECT ONSET GEOMETRY DOES NOT AFFECT CALORIMETRY Foil sample Pellet Sample Heat Flow (mw) Temperature ( C) o

26 SAMPLING VARIABLES SCANNING RATE SCAN RATE AFFECTS PEAK POSITION SCAN RATE DOES NOT AFFECT CALORIMETRY 100 Heat Flow (mw) o o o o o 1 C/min 5 C/min 10 C/min 20 C/min 40 C/min o Temperature ( C)

27 Specific Heat (J/g C) SAMPLE CONDITIONING Curve 1: DDSC File info: PET009 Thu Jan 12 11:08: Sample Weight: mg PET SCAN ISO # 1 PET SCAN ISO:PET009 Total C (J/g C) P # 2 PET SCAN ISO:PET007 Total C (J/g C) P Shock Cooled from the Melt 2. Cooled at 40 o C/min, then annealed at 70 o C. SAME SAMPLE, DIFFERENT THERMAL HISTORY AFTER 40 C/MIN COOL & Temperature ( C) BC PERKIN-ELMER 7 Series Thermal Analysis System Tue Jan 31 08:15:

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29 Sensor + Balance Quartz Purge in Sample in pan Microfurnace Thermocouple Purge out

30 Curve 1: TGA File info: wh-po Thu Sep 16 09:35: Sample Weight: mg white poly(ethylene) Onset C 80.0 Weight (Wt. %) n2-air TEMP1: 30.0 C TIME1: 0.0 min RATE1: 20.0 C/min TEMP2: C TIME2: 5.0 min Temperature ( C) roy PERKIN-ELMER 7 Series Thermal Analysis System Thu Aug 25 07:45:

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32 Curve 1: TGA File info: wh-po Thu Sep 16 09:35: Sample Weight: mg white poly(ethylene) # 1 white poly(ethylene):wh-po % Weight (Wt. %) # 2 black poly(ethylene):po0914b % Weight (Wt. %) Weight (Wt. %) n2-air TEMP1: 30.0 C TIME1: 0.0 min RATE1: 20.0 C/min TEMP2: C TIME2: 5.0 min Temperature ( C) roy PERKIN-ELMER 7 Series Thermal Analysis System Thu Aug 25 07:47:

33 Weight (Wt. %) Curve 1: TGA File info: rub5 Wed Jul 8 12:16: Sample Weight: mg Rubber step-wise Y Wt. % Y Wt. % Y Wt. % TEMP1: C TIME1: 0.0 min RATE1: C/min TEMP2: C TIME2: 3.0 min RATE2: C/min TEMP3: C TIME3: 3.0 min RATE3: C/min TEMP4: C Temperature ( C) BCassel PERKIN-ELMER 7 Series Thermal Analysis System Wed Aug 24 15:41:

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35 Penetration (mm) TMA Penetration Experiment Curve 1: TMA in Penetration File info: T5exx1 Wed Oct 4 16:18: Sample Height: mm POLYPROPYLENE BLEND Onset C TEMP1: C TIME1: 0.0 min RATE1: 10.0 C/min TEMP2: C Temperature ( C) B.TWOMBLY PERKIN-ELMER 7 Series Thermal Analysis System Tue Sep 6 14:59:

36 Expansion (mm) TMA Expansion Analysis Curve 1: TMA in Expansion File info: T5refE Tue Aug 29 16:43: Sample Height: mm REFERENCE MATERIAL E Cx x 10-4 /C Onset C Cx 2.75 x 10-5 /C ASTM D696 TEMP1: C TIME1: 0.0 min RATE1: 5.0 C/min TEMP2: C Temperature ( C) B.TWOMBLY PERKIN-ELMER 7 Series Thermal Analysis System Tue Sep 6 15:09:

37 Extension (mm) TMA Extension Experiment Curve 1: TMA in Extension File info: nylnextg Sun Aug 7 14:34: Sample Height: mm NYLON MONOFILEMENT INITIAL RUN TEMP1: C TIME1: 0.0 min RATE1: 5.0 C/min TEMP2: C Temperature ( C) B.Cassel PERKIN-ELMER 7 Series Thermal Analysis System Tue Sep 6 15:12:

38 DMA 7e Operation

39 The DMA 7e Can Perform Many Tests Temperature Scan Mode Isothermal (Time) Scan Mode Frequency Scan Mode Dynamic Stress Scan Mode Static Stress Scan Mode (Creep Ramp) Creep Analysis Stress Relaxation (Recovery Analysis) Creep-Recovery Analysis Constant Length Analysis (Shrinkage Force) Constant Force Analysis (TMA)

40 Perform many different types of tests melt, Tg, alpha, beta and gamma transitons, recrystallization, cure, modulus, damping, shrinkage, heat deflection, brittle point tests and many more...

41 Run many types of samples plastic, automotive, construction, aerospace, business products, metal, ceramic, food, cosmetic, environmental, biological materials.

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