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.
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.
Power Compensation DSC Quantitative DTA Measures dh directly Uses platinum resistance thermometers Derives dh Uses thermocouples
Temperature or Time
Effect of Sample Size on Sensitivity and Resolution 100 Indium Indium Indium 4.998 mg 10.001 mg 20.072 mg Peak = 158.93 Heat Flow (mw) 75 50 25 Peak from: to: Onset = J/g = Peak from: to: Onset = J/g = Peak from: to: Onset = J/g = 155.50 160.50 156.51 28.51 155.50 161.40 156.56 28.49 155.50 162.70 156.54 28.71 Peak = 158.30 Peak = 157.74 0 145.00 150.00 155.00 160.00 165.00 170.00 o Temperature ( C)
Heat Flow (mw) Curve 1: DSC File info: hdpe2 Thu Jul 12 14:18:44 1990 Sample Weight: 8.109 mg High Density Polyethylene @ 10C/min 40.0 35.0 30.0 X1 22.666 X2 135.000 Peak 127.373 Area 1611.915 mj H 198.781 J/g Height 23.315 mw Onset 118.769 C C C C 25.0 20.0 15.0 10.0 25.0 50.0 75.0 100.0 125.0 150.0 175.0 200.0 TEMP1: 15.0 C TIME1: 0.0 min RATE1: 10.0 C/min TEMP2: 200.0 C Temperature ( C) Application Laboratory PERKIN-ELMER 7 Series Thermal Analysis System Mon Aug 22 13:16:13 1994
Heat Flow (mw) Curve 1: DSC File info: polye Mon Jul 22 12:23:59 1985 Sample Weight: 14.273 mg POLYESTER INITIAL HEATING 60.0 55.0 # 1 POLYESTER INITIAL HEATING:polye Heat Flow (mw) # 2 POLYESTER AFTER QUENCHING FROM THE MELT Heat Flow (mw) 50.0 45.0 40.0 35.0 30.0 25.0 20.0 15.0 10.0 5.0 0.0-5.0-10.0 100.0 150.0 200.0 250.0 300.0 TEMP1: 40.0 C TIME1: 0.0 min RATE1: 40.0 C/min TEMP2: 300.0 C Temperature ( C) PERKIN-ELMER 7 Series Thermal Analysis System Mon Aug 22 13:40:34 1994
Heat Flow (mw) Analysis of Low Melting Wax Curve 1: DSC File info: dtc02 Mon Feb 20 16:12:35 1989 Sample Weight: 3.502 mg Dotriacontane 2 C/min 60.0 55.0 50.0 Peak 70.54 H 161.74 J/g C 45.0 Peak 65.49 H 60.02 J/g C 40.0 35.0 Onset 64.67 C Onset 69.23 C 30.0 58.0 62.0 66.0 70.0 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 13:47:18 1994
CALORIMETRY CONSIDERATIONS SAMPLING VARIABLES SAMPLE SIZE SAMPLE GEOMETRY SAMPLE PANS SAMPLE CONDITIONING
CALORIMETRY CONSIDERATIONS INSTRUMENTAL/TEST VARIABLES SCAN RATE PURGE GAS CALIBRATION COOLANT
Heat Flow (mw) CONSTANT CALORIMETRY REGARDLESS OF SAMPLE SIZE. Curve 1: DSC File info: indium004 Tue Feb 14 16:30:54 1995 Sample Weight: 4.998 mg Indium (4.998mg.) 100.0 90.0 80.0 70.0 60.0 50.0 Peak 158.66 H 28.52 J/g Indium 20.072 mg. C 40.0 30.0 Peak 157.92 Indium 10.002 mg. H 28.52 J/g C 20.0 10.0 Indium 4.998 mg. Peak 157.57 H 28.46 J/g C 0.0-10.0-20.0 Indium Onset 156.55 CIndium 4.998 4.998 mg. mg. Indium 10.002 mg. Onset 156.48 C Indium 20.072 mg. Onset 156.5 C 150.0 152.0 154.0 156.0 158.0 160.0 162.0 164.0 CALORIMETRIC TEST TEMP1: 140.0 C TIME1: 0.0 min RATE1: 10.0 C/min TEMP2: 175.0 C Temperature ( C) Tech.Support Lab PERKIN-ELMER 7 Series Thermal Analysis System Wed Feb 15 12:18:25 1995
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 150.0 Foil sample Pellet Sample 112.5 Heat Flow (mw) 75.0 37.5 341310 0.0 145.00 150.00 155.00 160.00 165.00 170.00 175.00 Temperature ( C) o
SAMPLING VARIABLES SCANNING RATE SCAN RATE AFFECTS PEAK POSITION SCAN RATE DOES NOT AFFECT CALORIMETRY 100 Heat Flow (mw) 75 50 o o o o o 1 C/min 5 C/min 10 C/min 20 C/min 40 C/min 25 0 154.00 156.00 158.00 160.00 162.00 164.00 166.00 341311 o Temperature ( C)
Specific Heat (J/g C) SAMPLE CONDITIONING Curve 1: DDSC File info: PET009 Thu Jan 12 11:08:23 1995 Sample Weight: 16.170 mg PET SCAN ISO 5.0 4.5 4.0 # 1 PET SCAN ISO:PET009 Total C (J/g C) P # 2 PET SCAN ISO:PET007 Total C (J/g C) P 3.5 3.0 2.5 2.0 1.5 1.0 0.5 0.0-0.5-1.0-1.5 1. Shock Cooled from the Melt 2. Cooled at 40 o C/min, then annealed at 70 o C. SAME SAMPLE, DIFFERENT 100.0 150.0 200.0 250.0 THERMAL HISTORY AFTER 40 C/MIN COOL & ANNEAL @65 Temperature ( C) BC PERKIN-ELMER 7 Series Thermal Analysis System Tue Jan 31 08:15:53 1995
Sensor + Balance Quartz Purge in Sample in pan Microfurnace Thermocouple Purge out
Curve 1: TGA File info: wh-po Thu Sep 16 09:35:25 1993 Sample Weight: 33.043 mg white poly(ethylene) 110.0 100.0 90.0 Onset 438.85 C 80.0 Weight (Wt. %) 70.0 60.0 50.0 40.0 30.0 20.0 10.0 0.0 100.0 200.0 300.0 400.0 500.0 600.0 n2-air TEMP1: 30.0 C TIME1: 0.0 min RATE1: 20.0 C/min TEMP2: 1000.0 C TIME2: 5.0 min Temperature ( C) roy PERKIN-ELMER 7 Series Thermal Analysis System Thu Aug 25 07:45:35 1994
Curve 1: TGA File info: wh-po Thu Sep 16 09:35:25 1993 Sample Weight: 33.043 mg white poly(ethylene) 100.0 # 1 white poly(ethylene):wh-po % Weight (Wt. %) # 2 black poly(ethylene):po0914b % Weight (Wt. %) 90.0 80.0 Weight (Wt. %) 70.0 60.0 50.0 40.0 30.0 20.0 10.0 0.0 200.0 400.0 600.0 800.0 1000.0 n2-air TEMP1: 30.0 C TIME1: 0.0 min RATE1: 20.0 C/min TEMP2: 1000.0 C TIME2: 5.0 min Temperature ( C) roy PERKIN-ELMER 7 Series Thermal Analysis System Thu Aug 25 07:47:28 1994
Weight (Wt. %) Curve 1: TGA File info: rub5 Wed Jul 8 12:16:42 1987 Sample Weight: 3.044 mg Rubber step-wise 100.0 90.0 Y -17.65 Wt. % 80.0 70.0 60.0 Y -44.95 Wt. % 50.0 40.0 30.0 20.0 Y -34.44 Wt. % 10.0 0.0 100.0 200.0 300.0 400.0 500.0 600.0 700.0 800.0 TEMP1: 100.0 C TIME1: 0.0 min RATE1: 100.0 C/min TEMP2: 325.0 C TIME2: 3.0 min RATE2: 100.0 C/min TEMP3: 500.0 C TIME3: 3.0 min RATE3: 100.0 C/min TEMP4: 900.0 C Temperature ( C) BCassel PERKIN-ELMER 7 Series Thermal Analysis System Wed Aug 24 15:41:32 1994
Penetration (mm) TMA Penetration Experiment Curve 1: TMA in Penetration File info: T5exx1 Wed Oct 4 16:18:08 1989 Sample Height: 1.354 mm POLYPROPYLENE BLEND 1.50 1.45 Onset 175.87 C 1.40 1.35 1.30 1.25 1.20 1.15 1.10 1.05 1.00 50.0 75.0 100.0 125.0 150.0 175.0 200.0 TEMP1: -125.0 C TIME1: 0.0 min RATE1: 10.0 C/min TEMP2: 250.0 C Temperature ( C) B.TWOMBLY PERKIN-ELMER 7 Series Thermal Analysis System Tue Sep 6 14:59:56 1994
Expansion (mm) TMA Expansion Analysis Curve 1: TMA in Expansion File info: T5refE Tue Aug 29 16:43:28 1989 Sample Height: 5.315 mm REFERENCE MATERIAL E 5.48 5.46 5.44 5.42 Cx 2.737 x 10-4 /C 5.40 5.38 5.36 Onset 137.08 C 5.34 5.32 Cx 2.75 x 10-5 /C 5.30-200.0-100.0 0.0 100.0 200.0 ASTM D696 TEMP1: -180.0 C TIME1: 0.0 min RATE1: 5.0 C/min TEMP2: 230.0 C Temperature ( C) B.TWOMBLY PERKIN-ELMER 7 Series Thermal Analysis System Tue Sep 6 15:09:24 1994
Extension (mm) TMA Extension Experiment Curve 1: TMA in Extension File info: nylnextg Sun Aug 7 14:34:43 1988 Sample Height: 8.640 mm NYLON MONOFILEMENT 13.0 12.0 11.0 10.0 9.0 8.0 7.0 6.0-50.0 0.0 50.0 100.0 150.0 200.0 INITIAL RUN TEMP1: -50.0 C TIME1: 0.0 min RATE1: 5.0 C/min TEMP2: 240.0 C Temperature ( C) B.Cassel PERKIN-ELMER 7 Series Thermal Analysis System Tue Sep 6 15:12:19 1994
DMA 7e Operation
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)
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...
Run many types of samples plastic, automotive, construction, aerospace, business products, metal, ceramic, food, cosmetic, environmental, biological materials.