Differential Scanning Calorimetry

● Used to understand amorphous and crystalline behavior

● Expected results
○ DSC results (onset, peak, end temperatures, and enthalpies
○ Heat capacity
■ Amount of energy a unit of matter can hold
■ From solid to liquid: heat capacity increases as the material becomes
solid, since it can hold more energy at the liquid state
■ As the heat capacity increases with temperature, there would be a slight
upward slope
○ Glass transition (temperature Tg)
■ Melting of amorphous material
■ Only for amorphous materials
■ No latent heat associated with it
■ Referred to as the second order transition
■ Amorphous material + heat = increase heat capacity (material gets
enough energy and becomes mobile)
■ Appears as a step change in the baseline
■ Changes due to either different degrees of polymerization or modification
of additives, physical properties of material changes
■ Baseline T increase < Tg < Tmelting
■ As the glass transition changes due to either different degrees of
polymerization or modification by additives, the physical properties of the
material change.

■
○ Tm
■ Where materials melt
 ■ For endotherms
● Equals to the peak temperature
■ Data you get
● Onset of melting
● Peak temperature
○ Peak melting temp
■ ICTAC standards say you should take the onset of
the melt peak as the melting point for metals,
organics, and similar materials, but the peak value
should be used for polymers.
■ complete melting in organics and the energy that
the melting transition needs in order to occur.
This is the enthalpy of the transitions and it is
associated with the crystallinity of materials.
■ A.k.a the enthalpy of transition
■ Associated with the crystallinity of materials
○ Crystallization Temperatures
■ an exothermic event where a liquid changes to a solid. This is depicted
as a peak. The extrapolated onset and peak temperature characterize
this event.
○ No enthalpy = amorphous (not crystalline)
● A sample of known mass is heated or cooled and the changes in its heat capacity
are tracked as changes in the heat flow
● This allows the detection of transitions like melts, glass transitions, phase changes,
and curing
○ For polymeric materials, the glass transition is important
● Literature: ratnayake 2006
● Sample DSC
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● Baka kaya wala na yung ibang peaks kasi hindi amorphous yung samples natin —
crystalline sila
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● More on data analysis of DSC results:
http://lipidlibrary.aocs.org/Biochemistry/content.cfm?ItemNumber=40884#data
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DSC of CS
DSC of RM

RVA
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● (From Cozzolino 2016^)
● Perten instruments

●
● ^ actual typical starch pasting profile
● Retrogradation
○ Related to the degree of stickiness of cooked grains
○ Network formation
● Long grains usually show high pasting temperature (PT) and low peak viscosity (PV)
○ Due to high amylose content
● Cold viscosity
○ Swelling of starch granules or products of high shear systems display elevated
viscosities
● Hot viscosity
○ Transition products
○ Reflects raw features or less cooked characteristics in a product
● Final viscosity
○ Set back
○ Gel set of the cooked RVA sample
○ Recombination of the starch in sample
● Gelatinization
○ Loss of crystalline order in starch lamellae
○ Onset of gelatinization
■ When the granules start to swell
● Pasting
○ Swelling, leaching or amylose, polymer alignment
○ Continuation of gelatinization
○ Phenomena following gelatinization in the dissolution of starch
○ Involves granular swelling (part of gelatinization)
○ Ease of pasting
■ How easy the starch is cooked
● RVA Graph
○ https://www.newfoodmagazine.com/article/15042/viscosity-measurements-food-p
roducts/
● Pasting temp
○ Temperature of infection point
○ Where viscosity starts to increase
● Peak time
○ Length of time from the beginning of heating until starch reaches maximum
viscosity
● Those with high amylose content, take a longer time to achieve the peak temperature
○ Expected it for our cornstarch materials
■ Though need to check
○ The amylose content indicates granule integrity
● Peak viscosity
○ Highest viscosity achieved
● Breakdown
 ○ Difference between peak viscosity and the viscosity measured in the valley
■ The valley would be the trough, in my understanding ito yung lowest point
○ A larger value indicates
■ Starch will lose its viscosity faster
■ Starch is not that stable
● Final viscosity
○ During cooling period
○ Where viscosity increases at cooling period
○ Retrogradation starts
■ Set back viscosity = final viscosity - peak temperature
● Correlates to cooked texture
● When the starch paste is cooled down, the onset of gelatinization
starts
● Measure the tendency of starch to undergo retrogradation
● They say that to compare results, the materials must have the same concentration,
heating time and temperature when done through RVA
○ Because a longer heating time and higher temperatures may increase the
viscosity of a material
● Pasting properties depends on the following
○ Time of heating
○ Temperature of heating
○ Shear
■ High amount of mixing and stirring during cooking, the faster the
gelatinization would start and be completed
○ pH
○ Ratio of the materials
○ Types of starch