SlideShare uma empresa Scribd logo
1 de 45
به نام خدا 
1
DSC 
Differential 
Scanning 
Calorimetry 
گرماسنجی افتراقی 
2 
Falsafi.r@gmail.com
Outlines 
• Introduction 
• DSC main parts 
- Pans - Purge gas - DSC cooling system 
• Sample preparation 
• DSC working principle 
• ICTA & anti ICTA 
• DSC curve 
• DSC types 
3
DSC 
Differential: measurement of the difference in temperature 
or heat flow from sample and reference side 
Scanning: the common operation mode is to run 
temperature or time scans 
Calorimeter: instrument to measure heat or heat flow. 
Heat flow: a transmitted power measured in mW 
4
• The reference pan is to remain empty at all times. 
• Signals from both pans provide information to the computer. This allows it to regulate the 
temperature and provide a constant heating rate. 
• time is heating rate dependent 
Metal 
1 
Metal 
2 
Metal 
1 
Metal 
2 
Sample Empty 
Sample 
Temperature 
Reference 
Temperature 
Temperature 
Difference 
• Different heating rate from 1 – 500̊C/min 
5 Danley, R. (2003)
melting 
In, 6.0000 mg 
mW 
0 
-10 
-20 
120 130 140 150 160 170 °C 
^exo 
STARe SW 9.10 
MSG Lab: NJ 
Heat flow 
Temperature or 
Time 
6
• made from gold, copper, aluminium, graphite and 
platinum, etc. 
• The lids can either provide a complete enclosure or 
can contain a pin hole to release the pressure that 
builds up inside. 
• Most samples can be run in non-hermetically sealed 
pans either uncovered. 
Al Pt alumina Ni Cu quartz 
Pan 
• Atmospheric interaction is optimised by using an open 
(uncovered) pan. 
• Sometimes pans coated with an inert fluorophosphates 
Layer. This coating renders the pans inert to many 
chemicals. 
* Care should be taken not to overfill the pan to the point that the sample spills when the pan is being sealed 7
purge gas 
• chemically inert gas such as Argon or nitrogen 
• continuously circulating throughout the cell and purge 
the base of the cell and remove any dust, moisture or 
other gases that may accumulated as a result of the 
pans being heated. 
• Nitrogen is most commonly used as a purge gas as it is 
• inexpensive, inert and easily available. 
• This purge gas gets heated before entering the cell in 
order to equilibrate its temperature with that in the 
cell. 
8
DSC cooling system 
Simple, Inexpensive and Easy to- Operate but have limited cooling capabilities 
- Intercoolers (green coolant similar to Freon) 
- like the freezer in a home 
- don’t require a lot of maintenance and provide excellent control, 
but have defined temperature limits. 
Lowest possible temperatures and fastest cooling rates 
Dallas, G. (2006) 
• Air 
• Chillers 
• Refrigerated Coolers 
• LN2 systems 
9
Some of More used chillers 
10 
170
0 5 10 15 20 25 
250 
200 
150 
100 
50 
0 
-50 
-100 
-150 
Air cooled 
Intracooler 
Liquid nitrogen 
Temperature [°C] 
Time [min] 
11
A little about software 
12
* A little about software 
13
14
Sample Preparation 
• Accurately-weigh samples (~3-20 mg) 
• Small sample pans (0.1 mL) of inert or treated metals (Al, Pt, Ni, 
etc.) 
• Several pan configurations, e.g., open, pinhole, or hermetically-sealed 
(airtight) pans 
• The same material and configuration should be used for the sample 
and the reference 
• Material should completely cover the bottom of the pan to ensure 
good thermal contact 
15 
Della Gatta, G. et al., (2006)
Sample Preparation : Shape 
• Keep sample as thin as possible (to minimise thermal 
gradients) 
• Cover as much of the pan bottom as possible 
• Samples should be cut rather than crushed to obtain a 
thin sample (better and more uniform thermal contact 
with pan) 
• Keep sample as thin as possible (to minimize thermal gradient) 
• Cover as much of the pan bottom as possible 
99 
* Small sample masses and low heating rates increase resolution 
16
DSC working principle 
17
DSC working principle 
Ice 
Air 
Ts Tr 
Hot Plate 
Heat the hot plate from -20 °C to 30 °C, 
18
Time 
or Tr 
Temperature 
Tr 
Ts 
Tf 
Time 
ΔT =Ts-Tr 
0 
-0.5 
Tf 
DSC raw signal 
19
DSC raw signal 
Time 
or Tr 
ΔT =Ts-Tr 
0 
-0.5 
Tf 
Time 
or Tr 
Heat flow (mW) 
0 
-10 
=ΔT/Rth 
Rth, thermal 
resistence of 
the system 
DSC signal,  
Peak integral -> ΔH 
ΔH 
20 
A normal DSC curve is not horizontal, its baseline shows a slope
Endothermic: 
Endothermic and exothermic effects 
When the sample absorbs energy, the enthalpy change is said to be endothermic. 
Processes such as melting, vaporization and gelatinization are endothermic. 
Exothermic: 
When the sample releases energy, the process is said to be exothermic. Processes 
such as crystallization and Gelation are exothermic. 
21
ICTAC (International Confederation for Thermal Analysis and Calorimetry) 
Direction of DSC signal 
melting 
In, 6.0000 mg 
mW 
0 
-10 
-20 
120 130 140 150 160 170 °C 
^exo 
STARe SW 9.10 
MSG Lab: NJ 
melting 
In, 6.0000 mg 
mW 
20 
15 
10 
5 
0 
120 130 140 150 160 170 °C 
^en do 
STARe SW 9 .1 0 
MSG L ab: NJ 
ICTA (ΔT=Ts-Tr) 
endothermic downwards 
exothermic upwards. 
Anti-ICTA (ΔT=Tr-Ts) 
endothermic upwards, 
exothermic downwards. 
ICTA and Anti-ICTA 
ˆexo ˆendo 
22
DSC Curve 
• The result of a DSC experiment is a curve of heat flux 
versus temperature or versus time. 
• This curve can be used to calculate enthalpies of transitions, 
which is done by integrating the peak corresponding to a 
given transition. 
• Area under the peak is directly proportional to heat 
absorbed or evolved by the reaction 
23 
melting 
In, 6.0000 mg 
mW 
20 
15 
10 
5 
0 
120 130 140 150 160 170 °C 
^en do
Factors affecting DSC curve 
• Two types of factors effect the DSC curve 
1-Instrumental factors 
• Furnace heating rate 
• Furnace atmosphere 
• Geometry of pan holder/location of sensors 
• Sensitivity of the recording system 
24
2- Sample characteristics 
• Amount of sample 
• Nature of sample 
• Solubility of evolved gases in the sample 
• Particle size 
• Thermal conductivity 
25
Influence of Sample Mass 
6 
150 152 154 156 
15mg 
Temperature (°C) 
0 
-2 
-4 
-6 
DSC Heat Flow (W/g) 
10mg 
4.0mg 
1.7mg 
1.0mg 
0.6mg 
Indium at 
10°C/minute 
Normalized Data 
Onset not 
influenced 
by mass 
158 160 162 164 166 
26
Effect of Heating Rate 
on Indium Melting Temperature 
6 
1 
0 
- 1 
- 2 
- 3 
- 4 
- 5 
154 156 158 160 162 164 166 168 170 
Temperature ( °C) 
Heat Flow (W/g) 
heating rates = 2, 5, 10, 20°C/min 
27
Factors affecting DSC curve 
28
29 
Different types of DSC
Heat Flux DSC 
Furnace 
• One block for both sample and reference cells 
• sample and reference are heated from the same source and the temperature difference ΔT 
is measured 
30 Danley, R. (2003)
Power Compensated DSC 
• sample and reference are heated by separate, individual heaters 
• temperature difference is kept close to zero, while the difference in the 
electrical power needed to maintain equal temperatures (ΔP = ΔQ/dt) is 
measured. 
31
Power Compensated Perkin Elmer DSC 1 
Differential Scanning Calorimter 
• Furnace 20 to 600°C 
• Maximum scan rate 500°C/min 
• Temperature Accuracy: ± 0.1°C 
• Sensitivity 0.1μW 
• Atmosphere nitrogen or air 
• Pyris software 
32
33
Modulated DSC 
• same heat flux DSC cell is used, but a sinusoidal temperature oscillation (modulation) is 
overlaid on the conventional linear temperature ramp 
• Two other factors: 
the amplitude of modulation 
and the period (frequency) of modulation 
• Separation of complex transition into more easily interpreted 
components 
• Increased sensitivity for detection of weak transitions 
• Increased resolution of transitions without loss of sensitivity 
• Increased accuracy in the measurement of polymer 
crystallinity 
34
Dynamic heating 
Types of DSC experiments 
Constant heat rate mode 
(e.g. heat flow vs. temperature) 
Isothermal Mode 
Done at constant temperature over a time period 
(e.g. heat flow vs. time) 
35
Glass Transition Temperature 
Crystallization 
Melting 
36
Definitions 
145 
125 
105 
85 
65 
45 
ΔT 
45 50 55 60 65 70 75 80 85 90 
Heat flow (mW) 
^Endo 
To 
Tc 
Tp 
ΔH = Area 
Interapolated baseline 
37
The Glass Transition Temperature 
38
Crystallization 
39
Melting 
40
Glass transition, crystallization and melting 
Glass transition 
Crystallization 
Melting 
Endo 
Putting it all together 
41
Parameters to control 
• Initial and final temperature 
• Heating or cooling rate 
• Amount of sample 
• Thermal history of sample 
• Type of gass: O2, N2, air 
• Gas flow rate 
* The general rule of thumb is that you should start your run at 20 ˚C below that expected temperature 
42
DSC Applications 
· Glass transition 
· Melting points 
· Crystallization times and 
temperatures 
· Heats of melting and crystallization 
· Percent crystallinity 
· Oxidative stabilities 
· Compositional analysis 
· Heat capacity 
· Purities 
· Thermal stabilities 
· Polymorphism 
43
44 
References 
Danley, R. New heat flux DSC measurement technique. Thermochimica Acta, 295, 201-208 (2003). 
Danley, R.L and Caulfield, P.A. DSC Baseline Improvements Obtained by a New Heat Flow Measurement 
Technique. TA Instruments, New Castle, DE 19720 (2001). 
Della Gatta, Giuseppe, Michael J. Richardson, Stefan M. Sarge, and Svein Stølen. "Standards, calibration, and 
guidelines in microcalorimetry. Part 2. Calibration standards for differential scanning calorimetry*(IUPAC Technical 
Report)." Pure and applied chemistry 78, no. 7 (2006): 1455-1476. 
Guide for choosing DSC pans. TA Instruments. Thermal applications note. TN-12. 
Menczel, J.D. Temperature calibration of heat flux DSC’s on cooling. J. Thermal Anal., 49, 193-199 (1997). 
M. J. Richardson, E. L. Charsley. “Calibration and standardisation in DSC”, in Handbook of 
Thermal Analysis and Calorimetry, P. K. Gallagher (Series Ed.), Vol. 1, “Principles and 
Practice”, M. E. Brown (Ed.), pp. 547–575(1998). 
Thermal Advantage Manual. DSC User Reference Guide . (TA Instruments, New Castle, DE.) (2000). 
Gide for running software. TA instrument. Theraml application note. TN-12. 
Dallas, G. Ph.D. and S. Aubuchon Ph.D. TA Instruments, 109 Lukens Drive, New Castle, DE 19720, USA (2006).
45 
Thank you…

Mais conteúdo relacionado

Mais procurados

DIFFERENTIAL THERMAL ANALYSIS (DTA), ppt
DIFFERENTIAL THERMAL ANALYSIS (DTA),  pptDIFFERENTIAL THERMAL ANALYSIS (DTA),  ppt
DIFFERENTIAL THERMAL ANALYSIS (DTA), pptshaisejacob
 
Thermal analysis - TGA & DTA
Thermal analysis - TGA & DTAThermal analysis - TGA & DTA
Thermal analysis - TGA & DTANaresh Babu
 
Differential thermal analysis - instrumental methods of analysis
Differential thermal analysis - instrumental methods of analysis Differential thermal analysis - instrumental methods of analysis
Differential thermal analysis - instrumental methods of analysis SIVASWAROOP YARASI
 
Thermal analysis by_menna_koriam
Thermal analysis by_menna_koriamThermal analysis by_menna_koriam
Thermal analysis by_menna_koriammennakoriam
 
Dsc: interpretaion and application
Dsc: interpretaion and applicationDsc: interpretaion and application
Dsc: interpretaion and applicationRahul Kumar Maurya
 
Thermal analysis and their application
Thermal analysis and their applicationThermal analysis and their application
Thermal analysis and their applicationyash prajapati
 
Presentation2dsc
Presentation2dscPresentation2dsc
Presentation2dscSrota Dawn
 
Thermal method of analysis
Thermal method of analysis Thermal method of analysis
Thermal method of analysis GANESH NIGADE
 
Differential Thermal Analysis(pdf)
Differential Thermal Analysis(pdf)Differential Thermal Analysis(pdf)
Differential Thermal Analysis(pdf)MayuriMore15
 
Differential thermal analysis
Differential thermal analysisDifferential thermal analysis
Differential thermal analysisSuresh Selvaraj
 
DIFFERENTIAL SCANNING CALORIMETRY(DSC)
DIFFERENTIAL SCANNING CALORIMETRY(DSC)DIFFERENTIAL SCANNING CALORIMETRY(DSC)
DIFFERENTIAL SCANNING CALORIMETRY(DSC)ArpitSuralkar
 
DIFFERENTIAL THERMAL ANALYSIS & DIFFERENTIAL SCANNING CALORIMETRY
DIFFERENTIAL THERMAL ANALYSIS & DIFFERENTIAL SCANNING CALORIMETRYDIFFERENTIAL THERMAL ANALYSIS & DIFFERENTIAL SCANNING CALORIMETRY
DIFFERENTIAL THERMAL ANALYSIS & DIFFERENTIAL SCANNING CALORIMETRYPrachi Pathak
 
Differential thermal analysis(dta)
Differential thermal analysis(dta)Differential thermal analysis(dta)
Differential thermal analysis(dta)Amruta Balekundri
 
Thermogravimetry Analysis (TGA)
Thermogravimetry Analysis (TGA)Thermogravimetry Analysis (TGA)
Thermogravimetry Analysis (TGA)Kalsoom Mohammed
 

Mais procurados (20)

Dta
DtaDta
Dta
 
DIFFERENTIAL THERMAL ANALYSIS (DTA), ppt
DIFFERENTIAL THERMAL ANALYSIS (DTA),  pptDIFFERENTIAL THERMAL ANALYSIS (DTA),  ppt
DIFFERENTIAL THERMAL ANALYSIS (DTA), ppt
 
Thermal analysis
Thermal analysisThermal analysis
Thermal analysis
 
TGA and DSC ppt
TGA and DSC ppt   TGA and DSC ppt
TGA and DSC ppt
 
Dta presentation
Dta presentationDta presentation
Dta presentation
 
Thermal analysis - TGA & DTA
Thermal analysis - TGA & DTAThermal analysis - TGA & DTA
Thermal analysis - TGA & DTA
 
Differential thermal analysis - instrumental methods of analysis
Differential thermal analysis - instrumental methods of analysis Differential thermal analysis - instrumental methods of analysis
Differential thermal analysis - instrumental methods of analysis
 
Thermal analysis by_menna_koriam
Thermal analysis by_menna_koriamThermal analysis by_menna_koriam
Thermal analysis by_menna_koriam
 
Dsc: interpretaion and application
Dsc: interpretaion and applicationDsc: interpretaion and application
Dsc: interpretaion and application
 
Thermal analysis and their application
Thermal analysis and their applicationThermal analysis and their application
Thermal analysis and their application
 
Presentation2dsc
Presentation2dscPresentation2dsc
Presentation2dsc
 
DSC and DTA
DSC and DTADSC and DTA
DSC and DTA
 
Thermal method of analysis
Thermal method of analysis Thermal method of analysis
Thermal method of analysis
 
Differential Thermal Analysis(pdf)
Differential Thermal Analysis(pdf)Differential Thermal Analysis(pdf)
Differential Thermal Analysis(pdf)
 
shiva ram
shiva ramshiva ram
shiva ram
 
Differential thermal analysis
Differential thermal analysisDifferential thermal analysis
Differential thermal analysis
 
DIFFERENTIAL SCANNING CALORIMETRY(DSC)
DIFFERENTIAL SCANNING CALORIMETRY(DSC)DIFFERENTIAL SCANNING CALORIMETRY(DSC)
DIFFERENTIAL SCANNING CALORIMETRY(DSC)
 
DIFFERENTIAL THERMAL ANALYSIS & DIFFERENTIAL SCANNING CALORIMETRY
DIFFERENTIAL THERMAL ANALYSIS & DIFFERENTIAL SCANNING CALORIMETRYDIFFERENTIAL THERMAL ANALYSIS & DIFFERENTIAL SCANNING CALORIMETRY
DIFFERENTIAL THERMAL ANALYSIS & DIFFERENTIAL SCANNING CALORIMETRY
 
Differential thermal analysis(dta)
Differential thermal analysis(dta)Differential thermal analysis(dta)
Differential thermal analysis(dta)
 
Thermogravimetry Analysis (TGA)
Thermogravimetry Analysis (TGA)Thermogravimetry Analysis (TGA)
Thermogravimetry Analysis (TGA)
 

Destaque

Ppp Dsc 1 Thermal Analysis Fundamentals Of Analysis
Ppp  Dsc 1 Thermal Analysis  Fundamentals Of AnalysisPpp  Dsc 1 Thermal Analysis  Fundamentals Of Analysis
Ppp Dsc 1 Thermal Analysis Fundamentals Of Analysisguest824336
 
3rd Year Undergraduate Cyclic Voltammetry Practical
3rd Year Undergraduate Cyclic Voltammetry Practical3rd Year Undergraduate Cyclic Voltammetry Practical
3rd Year Undergraduate Cyclic Voltammetry PracticalJames McAssey
 
Thermoanalytical techniques
Thermoanalytical techniquesThermoanalytical techniques
Thermoanalytical techniquesDeepali Jadhav
 
15ab1s0308
15ab1s030815ab1s0308
15ab1s03081918225
 
Thermal analysis
Thermal analysisThermal analysis
Thermal analysisceutics1315
 
Cyclic voltammetry
Cyclic voltammetryCyclic voltammetry
Cyclic voltammetryAfrin Nirfa
 
Differential thermal analysis & Differential Scanning Calorimetry
Differential thermal analysis & Differential Scanning CalorimetryDifferential thermal analysis & Differential Scanning Calorimetry
Differential thermal analysis & Differential Scanning Calorimetrysamira mohammadpour
 
Seminar on polymorphism
Seminar on polymorphismSeminar on polymorphism
Seminar on polymorphism023henil
 
Gas chromatography
Gas chromatographyGas chromatography
Gas chromatographybhavya mitta
 
Differential scanning calorimetry
Differential scanning calorimetryDifferential scanning calorimetry
Differential scanning calorimetryKhalid Hussain
 

Destaque (17)

DSC & TGA
DSC & TGA DSC & TGA
DSC & TGA
 
Cyclic Voltammetry
Cyclic VoltammetryCyclic Voltammetry
Cyclic Voltammetry
 
Ppp Dsc 1 Thermal Analysis Fundamentals Of Analysis
Ppp  Dsc 1 Thermal Analysis  Fundamentals Of AnalysisPpp  Dsc 1 Thermal Analysis  Fundamentals Of Analysis
Ppp Dsc 1 Thermal Analysis Fundamentals Of Analysis
 
3rd Year Undergraduate Cyclic Voltammetry Practical
3rd Year Undergraduate Cyclic Voltammetry Practical3rd Year Undergraduate Cyclic Voltammetry Practical
3rd Year Undergraduate Cyclic Voltammetry Practical
 
Thermoanalytical techniques
Thermoanalytical techniquesThermoanalytical techniques
Thermoanalytical techniques
 
15ab1s0308
15ab1s030815ab1s0308
15ab1s0308
 
Thermal analysis
Thermal analysisThermal analysis
Thermal analysis
 
Electrochemistry
ElectrochemistryElectrochemistry
Electrochemistry
 
Thermometiric titration
Thermometiric titrationThermometiric titration
Thermometiric titration
 
Cyclic voltammetry
Cyclic voltammetryCyclic voltammetry
Cyclic voltammetry
 
Thermometric titration
Thermometric titrationThermometric titration
Thermometric titration
 
Voltammetry
VoltammetryVoltammetry
Voltammetry
 
Differential thermal analysis & Differential Scanning Calorimetry
Differential thermal analysis & Differential Scanning CalorimetryDifferential thermal analysis & Differential Scanning Calorimetry
Differential thermal analysis & Differential Scanning Calorimetry
 
Seminar on polymorphism
Seminar on polymorphismSeminar on polymorphism
Seminar on polymorphism
 
Gas chromatography
Gas chromatographyGas chromatography
Gas chromatography
 
Differential scanning calorimetry
Differential scanning calorimetryDifferential scanning calorimetry
Differential scanning calorimetry
 
Gas chromatography
Gas chromatographyGas chromatography
Gas chromatography
 

Semelhante a Dsc instrument 1

diffrential scanning calorimetry is a barnch of analytical chemistry
diffrential scanning calorimetry is a barnch of analytical chemistrydiffrential scanning calorimetry is a barnch of analytical chemistry
diffrential scanning calorimetry is a barnch of analytical chemistryshamilfawasa
 
Differential Scanning Calorimetry (DSC).pdf
Differential Scanning Calorimetry (DSC).pdfDifferential Scanning Calorimetry (DSC).pdf
Differential Scanning Calorimetry (DSC).pdfSanDeepSharma926061
 
Presentation on DSC (differential scanning calorimetry )
Presentation on DSC (differential scanning calorimetry )Presentation on DSC (differential scanning calorimetry )
Presentation on DSC (differential scanning calorimetry )Hamza Suharwardi
 
DSC Chemical Presentation.ppt
DSC  Chemical Presentation.pptDSC  Chemical Presentation.ppt
DSC Chemical Presentation.pptMeet Zadafiya
 
thermaltechniquesdsc-190602083135.pdf
thermaltechniquesdsc-190602083135.pdfthermaltechniquesdsc-190602083135.pdf
thermaltechniquesdsc-190602083135.pdfKajalMIshra63
 
Differential scanning Colorimetry (DSC).
Differential scanning Colorimetry (DSC).Differential scanning Colorimetry (DSC).
Differential scanning Colorimetry (DSC).Poonam Aher Patil
 
Differentail scanning calorimtetery
Differentail scanning calorimteteryDifferentail scanning calorimtetery
Differentail scanning calorimteteryUroojAwan1
 
differential scanning calorimetry.pptx
differential scanning calorimetry.pptxdifferential scanning calorimetry.pptx
differential scanning calorimetry.pptxShashidarMShashi
 
Thermal techniques- DSC- Durgashree Diwakar
Thermal techniques- DSC- Durgashree DiwakarThermal techniques- DSC- Durgashree Diwakar
Thermal techniques- DSC- Durgashree DiwakarDurgashree Diwakar
 
DSC | DIFFERENTIAL SCANNING CALORIMETRY
DSC | DIFFERENTIAL SCANNING CALORIMETRYDSC | DIFFERENTIAL SCANNING CALORIMETRY
DSC | DIFFERENTIAL SCANNING CALORIMETRYKarthic27
 
Differential scanning calorimetry DSC
Differential scanning calorimetry DSCDifferential scanning calorimetry DSC
Differential scanning calorimetry DSCHaneenAbukatab
 
DSC- Basics PPT.ppt
DSC- Basics PPT.pptDSC- Basics PPT.ppt
DSC- Basics PPT.pptDHAYALK1
 
Differential scanning calorimeter dsc
Differential scanning calorimeter dscDifferential scanning calorimeter dsc
Differential scanning calorimeter dscHassan Alnajem
 
Thermo analytical methods by vsp
Thermo analytical methods by vspThermo analytical methods by vsp
Thermo analytical methods by vspVaishnavi Patil
 
abhishek 22mphyto13 term paper mpat.pptx
abhishek 22mphyto13 term paper mpat.pptxabhishek 22mphyto13 term paper mpat.pptx
abhishek 22mphyto13 term paper mpat.pptxAbhishekMahajan510050
 

Semelhante a Dsc instrument 1 (20)

diffrential scanning calorimetry is a barnch of analytical chemistry
diffrential scanning calorimetry is a barnch of analytical chemistrydiffrential scanning calorimetry is a barnch of analytical chemistry
diffrential scanning calorimetry is a barnch of analytical chemistry
 
Differential Scanning Calorimetry (DSC).pdf
Differential Scanning Calorimetry (DSC).pdfDifferential Scanning Calorimetry (DSC).pdf
Differential Scanning Calorimetry (DSC).pdf
 
Presentation on DSC (differential scanning calorimetry )
Presentation on DSC (differential scanning calorimetry )Presentation on DSC (differential scanning calorimetry )
Presentation on DSC (differential scanning calorimetry )
 
DSC Chemical Presentation.ppt
DSC  Chemical Presentation.pptDSC  Chemical Presentation.ppt
DSC Chemical Presentation.ppt
 
thermaltechniquesdsc-190602083135.pdf
thermaltechniquesdsc-190602083135.pdfthermaltechniquesdsc-190602083135.pdf
thermaltechniquesdsc-190602083135.pdf
 
Differential scanning Colorimetry (DSC).
Differential scanning Colorimetry (DSC).Differential scanning Colorimetry (DSC).
Differential scanning Colorimetry (DSC).
 
Differentail scanning calorimtetery
Differentail scanning calorimteteryDifferentail scanning calorimtetery
Differentail scanning calorimtetery
 
differential scanning calorimetry.pptx
differential scanning calorimetry.pptxdifferential scanning calorimetry.pptx
differential scanning calorimetry.pptx
 
Thermal techniques- DSC- Durgashree Diwakar
Thermal techniques- DSC- Durgashree DiwakarThermal techniques- DSC- Durgashree Diwakar
Thermal techniques- DSC- Durgashree Diwakar
 
DSC | DIFFERENTIAL SCANNING CALORIMETRY
DSC | DIFFERENTIAL SCANNING CALORIMETRYDSC | DIFFERENTIAL SCANNING CALORIMETRY
DSC | DIFFERENTIAL SCANNING CALORIMETRY
 
Thermal analysis 4
Thermal analysis  4Thermal analysis  4
Thermal analysis 4
 
Differential scanning calorimetry DSC
Differential scanning calorimetry DSCDifferential scanning calorimetry DSC
Differential scanning calorimetry DSC
 
DSC- Basics PPT.ppt
DSC- Basics PPT.pptDSC- Basics PPT.ppt
DSC- Basics PPT.ppt
 
Mahi
MahiMahi
Mahi
 
Differential scanning calorimeter dsc
Differential scanning calorimeter dscDifferential scanning calorimeter dsc
Differential scanning calorimeter dsc
 
thermal_properties..ppt
thermal_properties..pptthermal_properties..ppt
thermal_properties..ppt
 
UNIT 5 PPT.pptx
UNIT 5 PPT.pptxUNIT 5 PPT.pptx
UNIT 5 PPT.pptx
 
Thermo analytical methods by vsp
Thermo analytical methods by vspThermo analytical methods by vsp
Thermo analytical methods by vsp
 
abhishek 22mphyto13 term paper mpat.pptx
abhishek 22mphyto13 term paper mpat.pptxabhishek 22mphyto13 term paper mpat.pptx
abhishek 22mphyto13 term paper mpat.pptx
 
DSC.pdf
DSC.pdfDSC.pdf
DSC.pdf
 

Último

Reclaiming Pure Traditions Plants Enrichen Our Farms and Food.pdf
Reclaiming Pure Traditions Plants Enrichen Our Farms and Food.pdfReclaiming Pure Traditions Plants Enrichen Our Farms and Food.pdf
Reclaiming Pure Traditions Plants Enrichen Our Farms and Food.pdfStephen Gleave
 
Empowering Communities: Food Donation NGO Making a Difference
Empowering Communities: Food Donation NGO Making a DifferenceEmpowering Communities: Food Donation NGO Making a Difference
Empowering Communities: Food Donation NGO Making a DifferenceLovely Foundation
 
HOTMEN TAJUR BOGOR JAWA BARAT INDONESIAA
HOTMEN TAJUR BOGOR JAWA BARAT INDONESIAAHOTMEN TAJUR BOGOR JAWA BARAT INDONESIAA
HOTMEN TAJUR BOGOR JAWA BARAT INDONESIAAPermataAnnisa3
 
Beet Kvass The Probiotic-Rich, Fermented Tonic from Eastern Europe
Beet Kvass The Probiotic-Rich, Fermented Tonic from Eastern EuropeBeet Kvass The Probiotic-Rich, Fermented Tonic from Eastern Europe
Beet Kvass The Probiotic-Rich, Fermented Tonic from Eastern EuropeGarden Goddess, LLC
 
Food Supplement Directive No. 333-2020.pdf
Food Supplement Directive No. 333-2020.pdfFood Supplement Directive No. 333-2020.pdf
Food Supplement Directive No. 333-2020.pdfMohamed Miyir
 
Piping techniques in decorating cakes and cupcakes.
Piping techniques in decorating cakes and cupcakes.Piping techniques in decorating cakes and cupcakes.
Piping techniques in decorating cakes and cupcakes.Jolyn Sambrano
 
Explore The flavors Of Indian cuisine In Budapest : Indian Palate
Explore The flavors Of Indian cuisine In Budapest : Indian PalateExplore The flavors Of Indian cuisine In Budapest : Indian Palate
Explore The flavors Of Indian cuisine In Budapest : Indian PalateIndian Palate
 

Último (7)

Reclaiming Pure Traditions Plants Enrichen Our Farms and Food.pdf
Reclaiming Pure Traditions Plants Enrichen Our Farms and Food.pdfReclaiming Pure Traditions Plants Enrichen Our Farms and Food.pdf
Reclaiming Pure Traditions Plants Enrichen Our Farms and Food.pdf
 
Empowering Communities: Food Donation NGO Making a Difference
Empowering Communities: Food Donation NGO Making a DifferenceEmpowering Communities: Food Donation NGO Making a Difference
Empowering Communities: Food Donation NGO Making a Difference
 
HOTMEN TAJUR BOGOR JAWA BARAT INDONESIAA
HOTMEN TAJUR BOGOR JAWA BARAT INDONESIAAHOTMEN TAJUR BOGOR JAWA BARAT INDONESIAA
HOTMEN TAJUR BOGOR JAWA BARAT INDONESIAA
 
Beet Kvass The Probiotic-Rich, Fermented Tonic from Eastern Europe
Beet Kvass The Probiotic-Rich, Fermented Tonic from Eastern EuropeBeet Kvass The Probiotic-Rich, Fermented Tonic from Eastern Europe
Beet Kvass The Probiotic-Rich, Fermented Tonic from Eastern Europe
 
Food Supplement Directive No. 333-2020.pdf
Food Supplement Directive No. 333-2020.pdfFood Supplement Directive No. 333-2020.pdf
Food Supplement Directive No. 333-2020.pdf
 
Piping techniques in decorating cakes and cupcakes.
Piping techniques in decorating cakes and cupcakes.Piping techniques in decorating cakes and cupcakes.
Piping techniques in decorating cakes and cupcakes.
 
Explore The flavors Of Indian cuisine In Budapest : Indian Palate
Explore The flavors Of Indian cuisine In Budapest : Indian PalateExplore The flavors Of Indian cuisine In Budapest : Indian Palate
Explore The flavors Of Indian cuisine In Budapest : Indian Palate
 

Dsc instrument 1

  • 2. DSC Differential Scanning Calorimetry گرماسنجی افتراقی 2 Falsafi.r@gmail.com
  • 3. Outlines • Introduction • DSC main parts - Pans - Purge gas - DSC cooling system • Sample preparation • DSC working principle • ICTA & anti ICTA • DSC curve • DSC types 3
  • 4. DSC Differential: measurement of the difference in temperature or heat flow from sample and reference side Scanning: the common operation mode is to run temperature or time scans Calorimeter: instrument to measure heat or heat flow. Heat flow: a transmitted power measured in mW 4
  • 5. • The reference pan is to remain empty at all times. • Signals from both pans provide information to the computer. This allows it to regulate the temperature and provide a constant heating rate. • time is heating rate dependent Metal 1 Metal 2 Metal 1 Metal 2 Sample Empty Sample Temperature Reference Temperature Temperature Difference • Different heating rate from 1 – 500̊C/min 5 Danley, R. (2003)
  • 6. melting In, 6.0000 mg mW 0 -10 -20 120 130 140 150 160 170 °C ^exo STARe SW 9.10 MSG Lab: NJ Heat flow Temperature or Time 6
  • 7. • made from gold, copper, aluminium, graphite and platinum, etc. • The lids can either provide a complete enclosure or can contain a pin hole to release the pressure that builds up inside. • Most samples can be run in non-hermetically sealed pans either uncovered. Al Pt alumina Ni Cu quartz Pan • Atmospheric interaction is optimised by using an open (uncovered) pan. • Sometimes pans coated with an inert fluorophosphates Layer. This coating renders the pans inert to many chemicals. * Care should be taken not to overfill the pan to the point that the sample spills when the pan is being sealed 7
  • 8. purge gas • chemically inert gas such as Argon or nitrogen • continuously circulating throughout the cell and purge the base of the cell and remove any dust, moisture or other gases that may accumulated as a result of the pans being heated. • Nitrogen is most commonly used as a purge gas as it is • inexpensive, inert and easily available. • This purge gas gets heated before entering the cell in order to equilibrate its temperature with that in the cell. 8
  • 9. DSC cooling system Simple, Inexpensive and Easy to- Operate but have limited cooling capabilities - Intercoolers (green coolant similar to Freon) - like the freezer in a home - don’t require a lot of maintenance and provide excellent control, but have defined temperature limits. Lowest possible temperatures and fastest cooling rates Dallas, G. (2006) • Air • Chillers • Refrigerated Coolers • LN2 systems 9
  • 10. Some of More used chillers 10 170
  • 11. 0 5 10 15 20 25 250 200 150 100 50 0 -50 -100 -150 Air cooled Intracooler Liquid nitrogen Temperature [°C] Time [min] 11
  • 12. A little about software 12
  • 13. * A little about software 13
  • 14. 14
  • 15. Sample Preparation • Accurately-weigh samples (~3-20 mg) • Small sample pans (0.1 mL) of inert or treated metals (Al, Pt, Ni, etc.) • Several pan configurations, e.g., open, pinhole, or hermetically-sealed (airtight) pans • The same material and configuration should be used for the sample and the reference • Material should completely cover the bottom of the pan to ensure good thermal contact 15 Della Gatta, G. et al., (2006)
  • 16. Sample Preparation : Shape • Keep sample as thin as possible (to minimise thermal gradients) • Cover as much of the pan bottom as possible • Samples should be cut rather than crushed to obtain a thin sample (better and more uniform thermal contact with pan) • Keep sample as thin as possible (to minimize thermal gradient) • Cover as much of the pan bottom as possible 99 * Small sample masses and low heating rates increase resolution 16
  • 18. DSC working principle Ice Air Ts Tr Hot Plate Heat the hot plate from -20 °C to 30 °C, 18
  • 19. Time or Tr Temperature Tr Ts Tf Time ΔT =Ts-Tr 0 -0.5 Tf DSC raw signal 19
  • 20. DSC raw signal Time or Tr ΔT =Ts-Tr 0 -0.5 Tf Time or Tr Heat flow (mW) 0 -10 =ΔT/Rth Rth, thermal resistence of the system DSC signal,  Peak integral -> ΔH ΔH 20 A normal DSC curve is not horizontal, its baseline shows a slope
  • 21. Endothermic: Endothermic and exothermic effects When the sample absorbs energy, the enthalpy change is said to be endothermic. Processes such as melting, vaporization and gelatinization are endothermic. Exothermic: When the sample releases energy, the process is said to be exothermic. Processes such as crystallization and Gelation are exothermic. 21
  • 22. ICTAC (International Confederation for Thermal Analysis and Calorimetry) Direction of DSC signal melting In, 6.0000 mg mW 0 -10 -20 120 130 140 150 160 170 °C ^exo STARe SW 9.10 MSG Lab: NJ melting In, 6.0000 mg mW 20 15 10 5 0 120 130 140 150 160 170 °C ^en do STARe SW 9 .1 0 MSG L ab: NJ ICTA (ΔT=Ts-Tr) endothermic downwards exothermic upwards. Anti-ICTA (ΔT=Tr-Ts) endothermic upwards, exothermic downwards. ICTA and Anti-ICTA ˆexo ˆendo 22
  • 23. DSC Curve • The result of a DSC experiment is a curve of heat flux versus temperature or versus time. • This curve can be used to calculate enthalpies of transitions, which is done by integrating the peak corresponding to a given transition. • Area under the peak is directly proportional to heat absorbed or evolved by the reaction 23 melting In, 6.0000 mg mW 20 15 10 5 0 120 130 140 150 160 170 °C ^en do
  • 24. Factors affecting DSC curve • Two types of factors effect the DSC curve 1-Instrumental factors • Furnace heating rate • Furnace atmosphere • Geometry of pan holder/location of sensors • Sensitivity of the recording system 24
  • 25. 2- Sample characteristics • Amount of sample • Nature of sample • Solubility of evolved gases in the sample • Particle size • Thermal conductivity 25
  • 26. Influence of Sample Mass 6 150 152 154 156 15mg Temperature (°C) 0 -2 -4 -6 DSC Heat Flow (W/g) 10mg 4.0mg 1.7mg 1.0mg 0.6mg Indium at 10°C/minute Normalized Data Onset not influenced by mass 158 160 162 164 166 26
  • 27. Effect of Heating Rate on Indium Melting Temperature 6 1 0 - 1 - 2 - 3 - 4 - 5 154 156 158 160 162 164 166 168 170 Temperature ( °C) Heat Flow (W/g) heating rates = 2, 5, 10, 20°C/min 27
  • 30. Heat Flux DSC Furnace • One block for both sample and reference cells • sample and reference are heated from the same source and the temperature difference ΔT is measured 30 Danley, R. (2003)
  • 31. Power Compensated DSC • sample and reference are heated by separate, individual heaters • temperature difference is kept close to zero, while the difference in the electrical power needed to maintain equal temperatures (ΔP = ΔQ/dt) is measured. 31
  • 32. Power Compensated Perkin Elmer DSC 1 Differential Scanning Calorimter • Furnace 20 to 600°C • Maximum scan rate 500°C/min • Temperature Accuracy: ± 0.1°C • Sensitivity 0.1μW • Atmosphere nitrogen or air • Pyris software 32
  • 33. 33
  • 34. Modulated DSC • same heat flux DSC cell is used, but a sinusoidal temperature oscillation (modulation) is overlaid on the conventional linear temperature ramp • Two other factors: the amplitude of modulation and the period (frequency) of modulation • Separation of complex transition into more easily interpreted components • Increased sensitivity for detection of weak transitions • Increased resolution of transitions without loss of sensitivity • Increased accuracy in the measurement of polymer crystallinity 34
  • 35. Dynamic heating Types of DSC experiments Constant heat rate mode (e.g. heat flow vs. temperature) Isothermal Mode Done at constant temperature over a time period (e.g. heat flow vs. time) 35
  • 36. Glass Transition Temperature Crystallization Melting 36
  • 37. Definitions 145 125 105 85 65 45 ΔT 45 50 55 60 65 70 75 80 85 90 Heat flow (mW) ^Endo To Tc Tp ΔH = Area Interapolated baseline 37
  • 38. The Glass Transition Temperature 38
  • 41. Glass transition, crystallization and melting Glass transition Crystallization Melting Endo Putting it all together 41
  • 42. Parameters to control • Initial and final temperature • Heating or cooling rate • Amount of sample • Thermal history of sample • Type of gass: O2, N2, air • Gas flow rate * The general rule of thumb is that you should start your run at 20 ˚C below that expected temperature 42
  • 43. DSC Applications · Glass transition · Melting points · Crystallization times and temperatures · Heats of melting and crystallization · Percent crystallinity · Oxidative stabilities · Compositional analysis · Heat capacity · Purities · Thermal stabilities · Polymorphism 43
  • 44. 44 References Danley, R. New heat flux DSC measurement technique. Thermochimica Acta, 295, 201-208 (2003). Danley, R.L and Caulfield, P.A. DSC Baseline Improvements Obtained by a New Heat Flow Measurement Technique. TA Instruments, New Castle, DE 19720 (2001). Della Gatta, Giuseppe, Michael J. Richardson, Stefan M. Sarge, and Svein Stølen. "Standards, calibration, and guidelines in microcalorimetry. Part 2. Calibration standards for differential scanning calorimetry*(IUPAC Technical Report)." Pure and applied chemistry 78, no. 7 (2006): 1455-1476. Guide for choosing DSC pans. TA Instruments. Thermal applications note. TN-12. Menczel, J.D. Temperature calibration of heat flux DSC’s on cooling. J. Thermal Anal., 49, 193-199 (1997). M. J. Richardson, E. L. Charsley. “Calibration and standardisation in DSC”, in Handbook of Thermal Analysis and Calorimetry, P. K. Gallagher (Series Ed.), Vol. 1, “Principles and Practice”, M. E. Brown (Ed.), pp. 547–575(1998). Thermal Advantage Manual. DSC User Reference Guide . (TA Instruments, New Castle, DE.) (2000). Gide for running software. TA instrument. Theraml application note. TN-12. Dallas, G. Ph.D. and S. Aubuchon Ph.D. TA Instruments, 109 Lukens Drive, New Castle, DE 19720, USA (2006).