SOP (Standard Operating Procedure)

for the Perkin-Elmer Pyris 1 DSC

Tale of Contents
1! Preparing the DSC for operation
1!1 Turning on the system
1!" Checking the DSC configuration
1!"!1 Checking the DSC firm#are $ersion
1!"!" Checking the Pyris soft#are $ersion
1!% Connecting the peripheral gases
1!%!1 &itrogen gas
1!%!" 'elium gas
1!( )illing the cryofill
"! Operating the DSC
"!1 E*uilirating the DSC
"!" +aseline ad,ustment
"!% DSC caliration
"!%!1 Temperature caliration
"!%!" 'eat flo# caliration
"!%!% )urnace caliration
"!%!( Caliration reference materials
"!( -unning the DSC
"!(!1 Preparing the sample
"!(!" .nserting the sample into the DSC
"!(!% Programming your DSC run
"!(!( Starting and monitoring the DSC run
%! Post processing
%!1 +aseline correction
%!" Onset calculation
%!% Peak area calculation
%!( Specific heat calculation
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1. Preparing the DSC for operation
1.1 Turning on the system
Po#er up the system using the follo#ing steps /
(Step 1) Turn O& the computer
(Step ") Turn O& the
DSC y pressing the
s#itch on the rear panel
of the DSC as sho#n on
the right! .f the DSC
indicator panel is lit up
the DSC is O&!
(Step %) Turn O& the cryofill y pressing the s#itch on the cryofill control o0!
(&ote) Po#ered O& standy /
The entire system is usually kept O& e$en during standy! 'o#e$er1 you should e a#are that the
sample chamer may reach temperatures 2 (3 degC during non-operation!
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1.2 Checking the DSC configuration
4ou need to check the DSC configuration to ensure proper operation! T#o items need to e
confirmed1 the DSC firmware version and the Pyris software version!
1!"!1 Checking the DSC firm#are $ersion
.f you are certain that the firmware version is 6.4(or higher) skip this section!
The DSC firm#are $ersion can e checked y performing the follo#ing procedures /
(Step 1) )rom the 5indo#s desktop select /
Start - Programs - Pyris Software for !in"ows - Pyris Configuration
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(Step ") / The Pyris configuration #indo# #ill
appear as sho#n on the right! Comunication should
e #ith CO6" and the 78naly9ers: column should
display the Pyris 1 DSC as connected and
recogni9ed! )rom this screen1 press the #"it
utton!
(Step %) / The Pyris 1 DSC configuration #indo# #ill appear as sho#n elo#! 8t the time of
installation no gas accessories #ere included and the only checked o0 should e for the Cryofill!
Press the $irmware %ersion utton! 58-&.&; / Do &OT press the update )lash EP-O6 utton
unless you are attempting (after ha$ing consulted Perkin-Elmer) to re#rite the system:s )irm#are!
(Step () / The PyrisCfg #indo# should indicate that the
firm#are $ersion is version 6.4(or higher)! <ersion numer
is displayed as the last t#o digits of an unelie$aly long
garle of characters! .f the $ersion is incorrect1 you must
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update the firm#are after conferring #ith Perkin-Elmer and recei$ing ade*uate information on
performing the procedure correctly and safely!
(&otes) .nstallation history /
The Pyris 1 DSC #as installed in our la #ith the factory default firm#are $ersion =!3 and then
upgraded to $ersion =!( using a single floppy installation disk!
(&otes) Prolems #ith earlier )irm#are $ersions /
The only prolem noticed #ith older $ersions is a strange phantom glass transition #hich occurs at
around -1"> degC during measurements! This phantom change occurred e$en #hen the sample
pan #as empty! This can cause a sudden discontinuity in specific heat measurements efore and
after the none0istent transition!
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1!"!" Checking the Pyris soft#are $ersion
.f you are certain that the software version is &.'2(or higher) skip this section!
The Pyris soft#are communicates and controls the DSC from our computer! .t is also used for post-
processing pre$iously-performed DSC runs! The soft#are $ersion can e checked y performing
the follo#ing procedures /
(Step 1) )rom the 5indo#s desktop select /
Start - Programs - Pyris software for win"ows - Pyris (anager
(Step ") 8n emedded Pyris manager toolar #ill
appear on the screen! Press the Pyris 1 DSC utton!
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(Step %) The Pyris soft#are main #indo# #ill appear! 4ou should e ale to see the 7.nstrument
<ie#er: and 76ethod Editor: #indo#s inside the main #indo#! The 7Control Panel: should also e
emedded on the main #indo#!
(Step () )rom the main #indo# toolar1 select / )e*p - +,out-
8
(Step ?) The 8out Pyris #indo# should appear
and indicate the soft#are $ersion as &.'2(or
higher)! .f the $ersion is incorrect1 you must update
the soft#are after conferring #ith Perkin-Elmer and
recei$ing ade*uate information on performing the
procedure correctly and safely!
(&otes) .nstallation history /
The Pyris 1 DSC #as installed in our la #ith the factory default soft#are $ersion %!> and then
upgraded to $ersion %!>" using a single floppy installation disk!
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1.& Connecting the periphera* gases
Our DSC uses t#o types of gases during operation!
.itrogen gas is used as shield gas and is also supplied to
the cryofill! )e*ium gas is used as purge gas and is supplied
to the sample chamer! +oth gases pass through "rierite
columns to remo$e residual moisture!
1!%!1 &itrogen gas
.itrogen gas is pro$ided to oth the DSC shie*" gas inlet and the cryofi** gas inlet!
The supplied gas pressure should e 4/ psi!
There is a secon"ary pressure regu*ator et#een the drierite and the shield gas inlet #hich
controls the amount of gas flo# #hen the DSC slide co$er is opened! .f you feel the shield gas flo#
is inade*uate to pre$ent e0ternal moisture and particles from entering the sample holders1 increase
the flo# y turning the kno of the secondary regulator located on the rear corner of the DSC!
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1!%!" 'elium gas
)e*ium gas is pro$ided to the DSC purge inlet! The supplied gas pressure should e 20 psi!
(&ote) Do &OT use nitrogen gas for suamient DSC runs! &itrogen gas #ill li*uefy at
temperatures near -1@= degC or earlier!
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GAS FLOW
1.4 $i**ing the cryofi**
The cryofill needs to e filled #ith li*uid nitrogen using the follo#ing steps /
(Step 1) .f you ha$en:t done so already1 open the Pyris soft#are!
(Step ") Enale +OT' the shie*" gas and cover heater y pressing the
uttons on the Pyris control panel! Depressed uttons are at the O& state!
(Step %) Connect a li*uid nitrogen supply tank to the cryofill inlet $al$e using a cryo line(hose) ut
do not open any $al$es yet!
(Step () Open the cryofi** vent va*ve completely1 ut allo# the
$al$e to e loose and not completely e ,ammed in the
counterclock#ise direction! 4ou may ha$e difficulty closing the
$al$e if you do so due to ice formation around the $al$e
handle!
(Step ?) Open the cryofi** in*et va*ve va*ve completely1 ut
allo# the $al$e to e loose as descried ao$e!
(Step =) Open the li*uid nitrogen(A&") tank supply $al$e slo#ly
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and oser$e the pressure uildup in the cryofill! Pressure around 1 psi is normal1 ut should not
e0ceed 12 psi! .f the pressure is too high1 reduce the inflo# of A&" accordingly! 4ou #ill oser$e
nitrogen gas escaping through the cryofill $ent during the filling procedure! .f the cryofill #as empty
to egin #ith1 the hissing sound can ecome *uite loud! .t #ill recede #hen the cryofill has een
filled to a certain degree! 5hen the cryofill is almost completely filled1 2.2 wi** spora"ica**y ,urst
out from the $ent! This is a good time to end the filling as descried in the ne0t step! -ememer to
protect yourse*f from A&" free9e urns #ith cryo glo$es and protecti$e garments!
(Step >) Close the $al$es in the follo#ing order /
2.2 supp*y tank va*ve - Cryofi** in*et va*ve - Cryofi** vent va*ve
(Step B) 3mme"iate*y *oosen the cryo line(hose) to pre$ent pressure uild-up inside the line(hose)!
One usually maintains the connection on the cryofill inlet $al$e and loosens only the connection on
the A&" supply tank $al$e!
8ll preliminary setup is no# complete and the DSC is ready for operation!
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2. 4perating the DSC
2.1 #5ui*i,rating the DSC
The DSC needs to e filled #ith A&" from the cryofill prior to performing runs and measurements!
(Step 1) .f you ha$e not done so already1 turn O& all system components and open the Pyris
soft#are! See Chapter 1 for more information!
(Step ") 6ake sure the peripheral gases are eing supplied to the system and check the cryofill
le$el gauge to see if there is enough A&" for your runs and measurements!
(Step %) .f you ha$e not done so already1 enale +OT' the shie*" gas
and cover heater y pressing the uttons on the Pyris control panel!
Depressed uttons are at the O& state!
(Step () Enale the cryofi** utton on the Pyris control panel! The O& state #ill
indicate the cryofill utton in a +ACE color! The cryofill #ill no# start pumping A&" into
the DSC! .t takes at least " hours for the DSC to staili9e!
(&ote) .t is al#ays a good idea to pre$ent the sample
holder temperature from ecoming suamient during the
e*uiliration process! 4ou should monitor the temperature
eing displayed on the DSC indicator panel! .f the
temperature is ecoming too lo#1 set the furnace to heat
the sample holders manually y entering a
numer ("? degC is a good choice) in the
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input o0 of the control panel and then pressing the manua* go to temp utton!
2.2 6ase*ine a"7ustment
+aseline ad,ustment is performed to manually le$el the DSC cur$e and slope! .t should e
performed only #hen a sustantial change in the DSC hard#are component or system setup has
occurred! The ad,ustment procedure is composed of three steps /
D (anua* ,ase*ine optimi8ation
D 6ase*ine curvature correction
D 6ase*ine s*ope a"7ustment
)urther information concerning the procedure is a$ailale in the Pyris help module loaded on the
computer!
(&ote) +aseline correction /
+aseline correction is performed for most DSC runs using the Pyris soft#are during postprocessing!
This is due to the fact that the DSC thermogram cannot e completely le$el during the runs and #ill
e e0plained in the postprocessing section! 'o#e$er1 the soft#are aseline correction should not
e confused #ith the hard#are aseline ad,ustment descried ao$e!
2.& DSC ca*i,ration
Calirating the DSC consists of three components /
D Temperature ca*i,ration
D )eat f*ow ca*i,ration
D $urnace ca*i,ration
4ou should normally perform the calirations in the order descried ao$e! .t is especially important
to note that a furnace caliration should e done 8)TE- a temperature caliration!
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The caliration section descries procedures #ith #hich you may yet not e familiar #ith! -efer to
other portions of this document for the descried procedures as re*uired!
8ll sample measurements for caliration purposes should e repeated at least % times and
a$eraged1 using the run procedure you #ould normally use (cooling rate1 temperature range1 etc!)
"!%!1 Temperature caliration
1! 5hile in the .nstrument <ie#er or the 6ethod Editor1 select Calirate from the <ie# menu!
"! -estore the default Temperature caliration y selecting Temperature from the -estore
menu! .f you are performing all of the caliration procedures1 restore all default caliration
$alues y selecting the 8ll command!
%! Select the Save an" +pp*y utton in the Caliration #indo# to send the default caliration
$alues to the analy9er and sa$e the current caliration file!
(! Select C*ose to close the Caliration #indo#!
?! Complete a scan for each reference material under the same conditions that you run your
samples!
=! Perform a Peak 8rea calculation and include the Onset temperature! -ecord the E' (FGg)
and Onset resultsH you #ill need the Onset result for Temperature caliration and the E'
result for 'eat )lo# caliration!
>! -epeat steps ? and = for each additional reference material to e used!
B! Select the Calirate command in the %iew menu! The Caliration #indo# appears!
@! Select the Temperature ta! Enter the name of the reference material used1 the e0pected
Onset $alue1 and the Onset result ,ust measured for each reference material!
13! Select the check o0 in the Cse column for each reference material to e used in the
caliration!
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11! Select the Save an" +pp*y utton in the Caliration #indo# to send the ne# caliration
$alues to the analy9er and sa$e the current caliration file!
;o on to the ne0t caliration procedure y clicking on its ta or select C*ose to close the Caliration
#indo# and egin using the ne# caliration $alues!
"!%!" 'eat flo# caliration
1! 5hile using the .nstrument <ie#er or the 6ethod Editor1 select Calirate from the <ie#
menu!
"! -estore the default 'eat )lo# caliration y selecting 'eat )lo# from the -estore menu! .f
you performed a Temperature caliration ,ust prior to starting a 'eat )lo# caliration and
selected 8ll from the -estore menu1 then you do not need to restore the default 'eat )lo#
caliration here!
%! Select Save an" +pp*y!
(! Select C*ose!
?! Complete a scan using a reference material or use one that #as run for the Temperature
caliration!
=! Perform a Peak 8rea calculation and note the E' (FGg) result! 4ou can also use the E'
result recorded for one of the reference materials used in the Temperature caliration!
>! .n the .nstrument <ie#er or the 6ethod Editor1 select Calirate from the <ie# menu!
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B! Select the 'eat )lo# ta! .n the Caliration tale1 enter the name of the reference material
used1 the e0pected E' $alue1 the E' result ,ust measured1 the #eight of the reference
material used1 and the name of the method file used for the run!
@! Select the Save an" +pp*y utton in the Caliration #indo# to send the ne# caliration
$alue to the analy9er and sa$e the current caliration file!
;o on to the ne0t caliration procedure y clicking its ta or select C*ose to close the Caliration
#indo# and egin using the ne# caliration $alues!
"!%!% )urnace caliration
1! 5hile in the .nstrument <ie#er or the 6ethod Editor1 select Calirate from the <ie# menu!
"! .f applicale1 complete the Temperature caliration!
%! -emo$e the pans from sample and reference holders!
(! Select the )urnace ta in the Caliration #indo#!
?! .n the 6inimum field1 enter a minimum temperature that is elo# your normal operating
region!
=! .n the 6a0imum field1 enter a ma0imum temperature that is ao$e your normal operating
region!
>! Select the 6egin Ca*i,ration utton!
B! 5ait the designated time for completion of the )urnace caliration!
@! Select the Save an" +pp*y utton in the Caliration #indo# to send the ne# caliration
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$alues to the analy9er and sa$e the caliration file!
Select C*ose to close the Caliration #indo# and egin using the ne# caliration $alues!
"!%!( Caliration reference materials
<ery-high-purity (D@@!@@@I) organic materials can e used to calirate the temperature #hen
operating the DSC in the temperature range from J1>3KC! See the tale elo# for a list of
recommended suamient caliration standards that can e used #ith your DSC! &ormally1 the t#o
transition points of cyclohe0ane and the melting point of #ater is used for our purposes!

Su,stance Transition Transition Temp. 9KC: Transition #nergy 9;<g:
Cyclopentane Crystal J1?1!1= =@!(?
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Cyclopentane Crystal J1%?!3= (!@(
Cyc*ohe=ane Crystal JB>!3= >@!?B
Cyc*ohe=ane 6elt =!?( %1!"?
n-'eptane 6elt J@3!?= 1(3!1=
n-Octane 6elt J?=!>= 1B"!3
n-Decane 6elt J"@!== "3"!3@
&-Dodecane 6elt J@!=? "1=!>%
n-Octadecane 6elt "B!"( "(1!("
'e0atriacontane Crystal >"!1( 1B!>(
'e0atriacontane Crystal >%!B( =3!"?
'e0atriacontane 6elt >?!@( 1>?!%1
!ater 6elt 3!33
%%%!BB
1! The materials listed here1 if used for caliration1 must e of @@!@@@I minimum purity as
e$en small le$els of impurity can affect the temperature andGor energy of the transition!
"! .f the peaks are not sharp (as in indium)1 the sample may e impure and the temperatures
you measure may not e correct! Cse a higher purity sample or check the purity of the
sample y an alternate techni*ue such as gas chromatography!
2.4 >unning the DSC
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8fter the DSC has e*uilirated (usually more than " hours after cryofill has een enaled) you are
ready to perform DSC runs!
"!(!1 Preparing the sample
4ou #ill need to insert your sample for analysis into the DSC using sample pans! 8 nominal #eight
of ? mg (aout ? microliters) is a good amount of sample for analysis!
(Step 1) 6easure the sample pan lid (A)!
(Step ") 6easure the sample pan (P)!
(Step %) Place the sample into the sample pan and measure the #eight (PLS)! 6ake sure the
sample is distriuted e$enly along the ottom of the pan for est results!
(Step () Co$er the sample pan #ith the lid and crimp1 using the Perkin-Elmer crimp! -otate the
press handle until the press contacts the top of the lid! -otate the press handle an additional ">3
degrees to assure sealing #ithout e0cessi$e stress and deformation to the sample pan!
(Step ?) 6easure the total #eight of the sample pan (ALPLS)
(Step =) Determine the sample #eight (S) y t#o methods /
(PLS) J (P) and (ALPLS) J (A) J (P)
(Step >) 6ake sure the ao$e t#o $alues are #ithin 3!1 mg! .f not1 redo sample preparation #ith a
ne# pan!
(Step B) 8dditionaly1 prepare a reference sample pan #ith nothing inside it!
"!(!" .nserting the sample into the DSC
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(Step 1) Open the DSC s*i"e cover! The nitrogen shield gas should e flo#ing!
(Step ") -emo$e the platinum samp*e ho*"er covers using the DSC t#ee9er! Do not apply too
much force since this may cause the co$er holes to deform! Try not to scratch the co$ers1 either!
(Step %) .nsert the samp*e pan into the 2#$T sample holder1 and the reference 9empty: pan into
the >3?)T sample holder! Co$er the holders #ith their platinum sample co$ers and close the DSC
slide co$er!
"!(!% Programming your DSC run
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DSC Slide Cover
Sample Pa !oe" #ere
$e%ere&e Pa !oe" #ere
Program your run using the metho" e"itor!
(Step 1) Selecting the Samp*e 3nfo ta1 enter Sample .D1 Operator .D1 Comments1 and samp*e
weight! Csing the 6rowse utton1 determine the directory you #ish to sa$e your DSC run
information in1 and the filename!
(Step ") Selecting the 3nitia* State ta1 enter the necessary information as sho#n elo#!
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3nitia* temperature / temperature #here your run #ill start! Csually "? degC
@ 3nitia* / reference $alue of heat flo#! Csually 3!
Purge gas / Set as 'elium M "3 mlGmin
#5ui*i,rate temperature / Csually 3!31 degC
#5ui*i,rate heat f*ow / Csually 3!31 m5
#5ui*i,rate wait time / Csually 1? minutes
(Step %) Selecting the Program ta,1 enter the steps your run #ill consist of! 4our run #ill start #ith
an initial isothermal condition! Decide ho# long it #ill e isothermal in minute durations!
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(Step () Press +"" a step to include additional steps! Choose either Temperature Scan for
changing the temperature or 3sotherma* for maintaining a temperature!
(Step ?) .f you choose a Temperature Scan step1 input the target end temperature and the
coolingGheating rate!
25
(Step =) Select the #n" Con"ition utton to set ho# the system should eha$e after the run is
completed! The DSC temperature usually should return to its load temperature! 4ou can choose to
26
turn O)) the Cryofill and Co$er heater if you plan to e asent for a long time or if it:s your last run
for the day and you #on:t e ale to shut off the system #hen the run is completed! 4ou should
&OT opt to turn O)) the Cryofill if you plan to do another run! Turning O)) the cryofill #ill make an
e*uiliration period necessary #hen you re-enale the cryofill!
"!(!( Starting and monitoring the DSC run
27
Cse the 3nstrument %iewer #indo# to monitor the DSC! The 4-a0is displays the heat f*ow in
milli5atts and the N-a0is can display either the e*apse" time or temperature! The N-a0is display is
toggled using the TO-Dt toggle utton on the Pyris toolar!
The graph scale can automatically e ad,usted using the +utosca*e option under the %iew menu!
4ou can also manually change the scale of the 4 or N-a0is using the a0is scale uttons! 4ou can
further 9oom into a certain portion of the graph y clicking1 dragging1 and doule clicking on the
desired region!
5ait for the temperature and heat flo# to staili9e efore initiating your run! .t is a good idea to
manually set the temperature to the initial temperature of your run1 then #ait for staili9ation!
Staili9ation is normally assumed to ha$e een achie$ed #hen heat flo# oscillation is #ithin 3!31
milli5atts!
Start your run y pressing the DSC start utton! The run #ill start soon!
&. Post processing
28
Open your sa$ed data file! Select the portion of your run you #ish to analy9e y selecting the step
from the Curves - )eat $*ow menu! -emo$e the other residual data from the graph y selecting
the un#anted portion and pressing Shift-"e*ete!
&.1 6ase*ine correction
+aseline correction needs to e performed for most DSC runs using the Pyris soft#are due to the
fact that the DSC thermogram cannot e completely le$el during the runs! .n order to perform a
aseline correction1 you must /
(Step 1) Perform the same run performed for your sample1 ut #ith an empty sample pan and
setting the #eight as 3!
(Step ") Open the original sample run! Then add the empty sample run using the +"" "ata
function!
(Step %) Sutract the empty sample run from the original sample run using the (ath - Su,tract
function!
(Step () 4ou no# ha$e aseline-corrected thermogram data!
&.2 4nset ca*cu*ation
The onset calculation determines the eginning of any transition that is distinguished y a
significant change from the aseline! 8n e0ample of its use is the determination of the eginning of
a melt on a DSC heat flo# cur$e! 5hen you select 4nset from the Ca*c menu1 t#o A:s are
displayed on the acti$e cur$e and the dialog o0 appears/
- Aeft Aimit
Enter the left limit for the onset temperature calculation! 5hen the left limit is selected directly on
the cur$e y clicking on and dragging the leftmost A to the desired position1 the $alue in the entry
field automatically updates!
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- -ight Aimit
Enter the right limit for the onset temperature calculation! 5hen the right limit is selected directly
on the cur$e y clicking on and dragging the rightmost A to the desired position1 the $alue in the
entry field automatically updates!
- Calculate
Closes the dialog o01 displays tangents lines on the cur$e1 and displays the 8d,ust Tangents
dialog o0!
- Aeft Tangent radio utton (on 8d,ust Tangents dialog o0)
8cti$ates the left tangent for ad,ustment! .n general1 the left tangent corresponds to the point
#here the cur$e egins to de$iate from the aseline! Cse the Cp and Do#n uttons to ad,ust the
left tangent line or mo$e the line on the graph!
- -ight Tangent radio utton (on 8d,ust Tangents dialog o0)
8cti$ates the right tangent for ad,ustment! )or an onset calculation for a typical heating cur$e1 the
right tangent corresponds to the point of ma0imum slope of the leading edge of the peak! )or a
glass transition calculation1 the right tangent should e placed at a position on the cur$e #here
there is not much acti$ity since glass transition measures the change in specific heat! )or a step
transition calculation1 the right tangent should e #here the cur$e starts to go to ack to aseline!
Cse the Cp and Do#n uttons to ad,ust the right tangent line or mo$e the line on the graph!
- Calculate (on 8d,ust Tangents dialog o0)
8fter ad,usting the tangents1 click on Calculate to close the dialog o01 complete the calculation1
and display the results on the cur$e!
&.& Peak area ca*cu*ation
The peak area calculation determines the area1 starting point1 midpoint1 and end point of a peak
transition! .n heat flo# cur$es1 peak transitions are associated #ith melting1 crystalli9ation1 and
curing!
30
5hen you select Peak +rea from the Ca*c menu1 the Peak Calculation dialog o0 appears along
#ith t#o A:s! 4ou can use the mouse to drag the APs to the desired location on the peak to set the
limits of the calculation or you can use the keyoard to type in the limits! The limits should
completely encompass the peak transition! Cse the dialog o0 as follo#s/
- Aeft Aimit
Enter the left limit for the calculation! 5hen the left limit is selected directly on the cur$e y
clicking on and dragging the leftmost A to the desired position1 the $alue in the entry field
automatically updates!
- -ight Aimit
Enter the right limit for the calculation! 5hen the right limit is selected directly on the cur$e y
clicking on and dragging the rightmost A to the desired position1 the $alue in the entry field
automatically updates!
- +aseline
8fter setting the limits1 select the type of aseline to e used in the calculation and displayed /
Stan"ar" is a straight1 limit to limit aseline!
Sigmoi"a* aseline can e used #hen the cur$e efore the transition is at a different le$el than it
is after the transition! This most commonly occurs in heat flo# data! 5hen sigmoidal aseline is
chosen1 tangents are dra#n from the eginning of each specified limit! 4ou can ad,ust these
efore the calculation is performed! .t is recommended that you use the sigmoidal option!
- Other options to include for calculation and display
The 4nset $alue is calculated y finding the intersection of the aseline and the e0trapolated
tangent at the inflection point of the leading edge of the peak! The #n" $alue is calculated y
finding the intersection of the aseline and the e0trapolated tangent at the inflection point of the
trailing edge of the peak! The Peak )eight is the distance from the aseline to the peak! 4ou can
select one1 t#o1 or all three items! Select Disp*ay 2imits to ha$e the N14 $alues of the left and
right limits also displayed on the cur$e!
- 8rea Options
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Select B +rea Curve to calculate and display a percent area cur$e ased on the peak area
calculation!
&.4 Specific heat ca*cu*ation
.n order to perform a specific heat calculation you must /
- Perform a sample run 8&D an empty pan run #hich are identical in programmed steps
- 8ll temperature scan steps must e precluded and concluded #ith an isothermal step
(e0) iso M "?C -D Cool to -"?C M ?QGmin -D iso M -"?C -D Cool to ->?C M ?QGmin -D iso R!!
- The temperature scan steps must not e0ceed ?3 degC! That is1 the temperature difference from
eginning to end must not e0ceed ?3 degC in order to perform accurate Cp calculations!
- -ememer that specific heat cannot e correctly calculated if a phase change or reaction occurs
in that temperature region! 4ou must 7cut out: such regions y placing isotherms on either side!
(Step 1) 8fter data collection is complete1 click on the Data +na*ysis utton on the toolar!
(Step ") Open the sample data! Then add the aseline(empty pan) data using +"" Data in the $i*e
menu!
(Step %) Select the sample cur$e #ith your mouse! .f it ecomes the acti$e cur$e1 it #ill e displayed
#ith a hea$y line!
(Step () Click on )eat f*ow in the Curves menu! Select the desired temperature scan step 8&D the
isotherm steps efore and after the desired step!
(Step ?) Select the aseline(empty pan) cur$e #ith your mouse! .f it ecomes the acti$e cur$e1 it #ill
e displayed #ith a hea$y line!
(Step =) Click on )eat f*ow in the Curves menu! Select the desired temperature scan step 8&D the
isotherm steps efore and after the desired step!
(Step >) 4our thermogram #ill no# sho# a segment of the sample cur$e you #ish to analy9e and its
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corresponding aseline segment! Once again select the sample cur$e!
(Step B) Choose 6ultiple cur$e from the Specific heat sumenu under the Calc menu /
Ca*c - Specific heat - (u*tip*e curve
The default selection for the aseline cur$e should e the segment of the cur$e that
coincides #ith the segment of the sample cur$e selected! Click on OQ or press Enter to
accept the selection!
The specific heat cur$e and its ordinate scale should no# ha$e een added to the display!
-epeat steps % to B for other segments of your cur$e you #ish to analy9e!
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