Influence of the Processes Parameters on the Properties of The ...
Influence of the Processes Parameters on the Properties of The ...
Influence of the Processes Parameters on the Properties of The ...
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Chapter 4.<br />
Experimental Procedures and Protocols for Analyses<br />
3.2 Differential Scanning Calorimetry<br />
<strong>The</strong> transiti<strong>on</strong> temperature and change in specific heat capacity were measured by a NETZSCH<br />
DSC 204 Phoenix ® Set Up under a N 2 atmosphere. <strong>The</strong> DSC measuring cell c<strong>on</strong>sists <str<strong>on</strong>g>of</str<strong>on</strong>g> a cylindrical highc<strong>on</strong>ductivity<br />
silver block with an embedded heating coil for broad <str<strong>on</strong>g>the</str<strong>on</strong>g>rmal symmetry (3D symmetry) in <str<strong>on</strong>g>the</str<strong>on</strong>g><br />
sample chamber, <str<strong>on</strong>g>the</str<strong>on</strong>g> cooling ports for liquid nitrogen or compressed air cooling and a cooling ring for<br />
c<strong>on</strong>necti<strong>on</strong> <str<strong>on</strong>g>of</str<strong>on</strong>g> <str<strong>on</strong>g>the</str<strong>on</strong>g> intra-cooler (also with simultaneous liquid nitrogen cooling).<br />
For all <str<strong>on</strong>g>the</str<strong>on</strong>g> experiments, 3 – 10 mg were accurately weighed by a digital microbalance and sealed<br />
into an aluminium sample pan (pans are crimped close with sample press). An empty aluminium pan was<br />
used as <str<strong>on</strong>g>the</str<strong>on</strong>g> reference sample. <strong>The</strong> DSC heating and cooling rates were c<strong>on</strong>trolled at 10°C/min, and all<br />
experiments were carried out under a nitrogen purge.<br />
Following steps are made during <str<strong>on</strong>g>the</str<strong>on</strong>g> analysis,<br />
‣ Calibrating <str<strong>on</strong>g>the</str<strong>on</strong>g> instrument with indium<br />
‣ Selecting <str<strong>on</strong>g>the</str<strong>on</strong>g> pan type and material and preparing <str<strong>on</strong>g>the</str<strong>on</strong>g> sample<br />
‣ Creating or choosing <str<strong>on</strong>g>the</str<strong>on</strong>g> test procedure and entering sample and instrument informati<strong>on</strong> through <str<strong>on</strong>g>the</str<strong>on</strong>g><br />
TA instrument c<strong>on</strong>trol s<str<strong>on</strong>g>of</str<strong>on</strong>g>tware<br />
‣ Setting <str<strong>on</strong>g>the</str<strong>on</strong>g> purge gas flow rate, <str<strong>on</strong>g>the</str<strong>on</strong>g>n loading <str<strong>on</strong>g>the</str<strong>on</strong>g> sample and closing <str<strong>on</strong>g>the</str<strong>on</strong>g> cell lid<br />
‣ Starting <str<strong>on</strong>g>the</str<strong>on</strong>g> experiment and <str<strong>on</strong>g>the</str<strong>on</strong>g>n obtaining <str<strong>on</strong>g>the</str<strong>on</strong>g> data and <str<strong>on</strong>g>the</str<strong>on</strong>g>rmograms.<br />
Schematic presentati<strong>on</strong> <str<strong>on</strong>g>of</str<strong>on</strong>g> <str<strong>on</strong>g>the</str<strong>on</strong>g> <str<strong>on</strong>g>the</str<strong>on</strong>g>rmal analysis is presented in Figure 4.19<br />
B<br />
Compressed<br />
sample pan<br />
C<br />
Sample data<br />
Furnace program<br />
screen<br />
Aluminum<br />
pan press<br />
Aluminum<br />
top lid<br />
Tweezers<br />
Reference cup<br />
Liquid<br />
N 2 tank<br />
DSC sample chamber<br />
Test start<br />
window<br />
Experimental curve<br />
Aluminum<br />
base pan<br />
A<br />
DSC sample preparing<br />
accessories<br />
NETZSCH DSC 204 Phoenix® Set Up<br />
D<br />
Foam<br />
E<br />
Computer display and<br />
m<strong>on</strong>itoring unit<br />
Balance to weigh sample<br />
Polymer<br />
powder<br />
<strong>The</strong>rmogram with T g<br />
Figure 4.19: DSC analysis flow sheet <str<strong>on</strong>g>of</str<strong>on</strong>g> polymer material and foam.<br />
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