SOP (Standard Operating Procedure) for the Perkin-Elmer Pyris 1 DSC

Ta le 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*uili rating the DSC "!" +aseline ad,ustment "!% DSC cali ration "!%!1 Temperature cali ration "!%!" 'eat flo# cali ration "!%!% )urnace cali ration "!%!( Cali ration 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

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& stand y / The entire system is usually kept O& e$en during stand y! 'o#e$er1 you should e a#are that the sample cham er may reach temperatures 2 (3 degC during non-operation!

1.2 Checking the DSC configuration

4ou need to check the DSC configuration to ensure proper operation! T#o items need to confirmed1 the DSC firmware version and the Pyris software version! e

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

(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 $ersion is version 6.4(or higher)! <ersion num er is displayed as the last t#o digits of an un elie$a ly long gar le of characters! .f the $ersion is incorrect1 you must

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) Pro lems #ith earlier )irm#are $ersions / The only pro lem 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!

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 postprocessing 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 em edded Pyris manager tool ar #ill appear on the screen! Press the Pyris 1 DSC utton!

(Step %) The Pyris soft#are main #indo# #ill appear! 4ou should e a le to see the 7.nstrument <ie#er: and 76ethod Editor: #indo#s inside the main #indo#! The 7Control Panel: should also e em edded on the main #indo#!

(Step () )rom the main #indo# tool ar1 select / )e*p - +,out-

(Step ?) The 8 out 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!

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 cham er! +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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GAS FLOW

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 su am ient DSC runs! &itrogen gas #ill li*uefy at temperatures near -1@= degC or earlier!

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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 ") Ena le +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 allo# the $al$e to e loose as descri ed a o$e!

ut

(Step =) Open the li*uid nitrogen(A&") tank supply $al$e slo#ly

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and o ser$e the pressure uildup in the cryofill! Pressure around 1 psi is normal1 ut should not e0ceed 12 psi! .f the pressure is too high1 reduce the inflo# of A&" accordingly! 4ou #ill o ser$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 $ent! This is a good time to end the filling as descri ed in the ne0t step! -emem er to protect yourse*f from A&" free9e urns #ith cryo glo$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 ena le +OT' the shie*" gas and cover heater y pressing the uttons on the Pyris control panel! Depressed uttons are at the O& state! (Step () Ena le 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 sta ili9e! (&ote) .t is al#ays a good idea to pre$ent the sample holder temperature from ecoming su am ient during the e*uili ration 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 num er ("? 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 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$aila le in the Pyris help module loaded on the computer! (&ote) +aseline correction / +aseline correction is performed for most DSC runs using the Pyris soft#are during postprocessing! This is due to the fact that the DSC thermogram cannot e completely le$el during the runs and #ill e e0plained in the postprocessing section! 'o#e$er1 the soft#are aseline correction should not e confused #ith the hard#are aseline ad,ustment descri ed a o$e! e performed only #hen a su stantial change in the DSC hard#are component or system setup has

2.& DSC ca*i,ration

Cali rating the DSC consists of three components / D Temperature ca*i,ration D )eat f*ow ca*i,ration D $urnace ca*i,ration 4ou should normally perform the cali rations in the order descri ed a o$e! .t is especially important to note that a furnace cali ration should e done 8)TE- a temperature cali ration!

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The cali ration section descri es procedures #ith #hich you may yet not e familiar #ith! -efer to other portions of this document for the descri ed procedures as re*uired! 8ll sample measurements for cali ration 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 cali ration

1! 5hile in the .nstrument <ie#er or the 6ethod Editor1 select Cali rate from the <ie# menu! "! -estore the default Temperature cali ration y selecting Temperature from the -estore menu! .f you are performing all of the cali ration procedures1 restore all default cali ration $alues y selecting the 8ll command! %! Select the Save an" +pp*y utton in the Cali ration #indo# to send the default cali ration $alues to the analy9er and sa$e the current cali ration file! (! Select C*ose to close the Cali ration #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 cali ration and the E' result for 'eat )lo# cali ration! >! -epeat steps ? and = for each additional reference material to e used! B! Select the Cali rate command in the %iew menu! The Cali ration #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 cali ration!

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11! Select the Save an" +pp*y utton in the Cali ration #indo# to send the ne# cali ration $alues to the analy9er and sa$e the current cali ration file! ;o on to the ne0t cali ration procedure y clicking on its ta or select C*ose to close the Cali ration #indo# and egin using the ne# cali ration $alues!

"!%!" 'eat flo# cali ration

1! 5hile using the .nstrument <ie#er or the 6ethod Editor1 select Cali rate from the <ie# menu! "! -estore the default 'eat )lo# cali ration y selecting 'eat )lo# from the -estore menu! .f you performed a Temperature cali ration ,ust prior to starting a 'eat )lo# cali ration and selected 8ll from the -estore menu1 then you do not need to restore the default 'eat )lo# cali ration 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 cali ration! =! 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 cali ration! >! .n the .nstrument <ie#er or the 6ethod Editor1 select Cali rate from the <ie# menu!

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B! Select the 'eat )lo# ta ! .n the Cali ration ta le1 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 Cali ration #indo# to send the ne# cali ration $alue to the analy9er and sa$e the current cali ration file! ;o on to the ne0t cali ration procedure y clicking its ta or select C*ose to close the Cali ration #indo# and egin using the ne# cali ration $alues!

"!%!% )urnace cali ration

1! 5hile in the .nstrument <ie#er or the 6ethod Editor1 select Cali rate from the <ie# menu! "! .f applica le1 complete the Temperature cali ration! %! -emo$e the pans from sample and reference holders! (! Select the )urnace ta in the Cali ration #indo#! ?! .n the 6inimum field1 enter a minimum temperature that is elo# your normal operating region! =! .n the 6a0imum field1 enter a ma0imum temperature that is a o$e your normal operating region! >! Select the 6egin Ca*i,ration utton! B! 5ait the designated time for completion of the )urnace cali ration! @! Select the Save an" +pp*y utton in the Cali ration #indo# to send the ne# cali ration

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$alues to the analy9er and sa$e the cali ration file! Select C*ose to close the Cali ration #indo# and egin using the ne# cali ration $alues!

"!%!( Cali ration reference materials

<ery-high-purity (D@@!@@@I) organic materials can e used to cali rate the temperature #hen operating the DSC in the temperature range from J1>3KC! See the ta le elo# for a list of recommended su am ient cali ration 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 Cyclopentane

Transition Crystal

Transition Temp. 9KC: J1?1!1=

Transition #nergy 9;<g: =@!(?

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Cyclopentane Cyc*ohe=ane Cyc*ohe=ane n-'eptane n-Octane n-Decane &-Dodecane n-Octadecane 'e0atriacontane 'e0atriacontane 'e0atriacontane !ater

Crystal Crystal 6elt 6elt 6elt 6elt 6elt 6elt Crystal Crystal 6elt 6elt

J1%?!3= JB>!3= =!?( J@3!?= J?=!>= J"@!== J@!=? "B!"( >"!1( >%!B( >?!@( 3!33

(!@( >@!?B %1!"? 1(3!1= 1B"!3 "3"!3@ "1=!>% "(1!(" 1B!>( =3!"? 1>?!%1

%%%!BB 1! The materials listed here1 if used for cali ration1 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*uili rated (usually more than " hours after cryofill has een ena led) 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 (a out ? 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 distri uted 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$e stress and deformation to the sample pan! (Step ?) 6easure the total #eight of the sample pan (ALPLS) (Step =) Determine the sample #eight (S) y t#o methods / (PLS) J (P) and (ALPLS) J (A) J (P) (Step >) 6ake sure the a o$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!

DSC Slide Cover

Sample Pa

!oe" #ere

$e%ere &e Pa

!oe" #ere

"!(!% Programming your DSC run

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Program your run using the metho" e"itor! (Step 1) Selecting the Samp*e 3nfo ta 1 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 ta 1 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!

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(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

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turn O)) the Cryofill and Co$er heater if you plan to e a sent for a long time or if it:s your last run for the day and you #on:t e a le 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*uili ration period necessary #hen you re-ena le the cryofill!

"!(!( Starting and monitoring the DSC run

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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 tool ar! 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 dou le clicking on the desired region! 5ait for the temperature and heat flo# to sta ili9e efore initiating your run! .t is a good idea to manually set the temperature to the initial temperature of your run1 then #ait for sta ili9ation! Sta ili9ation 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

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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$el during the runs! .n order to perform a aseline correction1 you must / (Step 1) Perform the same run performed for your sample1 setting the #eight as 3! (Step ") Open the original sample run! Then add the empty sample run using the +"" "ata function! (Step %) Su tract the empty sample run from the original sample run using the (ath - Su,tract function! (Step () 4ou no# ha$e aseline-corrected thermogram data! ut #ith an empty sample pan and

&.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!

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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 key oard 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$e automatically updates! - -ight Aimit Enter the right limit for the calculation! 5hen the right limit is selected directly on the cur$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! y clicking on and dragging the leftmost A to the desired position1 the $alue in the entry field

- 8rea Options

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Select B +rea Curve to calculate and display a percent area cur$e calculation!

ased on the peak area

&.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! - -emem er 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 tool ar! (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 su menu under the Calc menu / Ca*c - Specific heat - (u*tip*e curve The default selection for the 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$e you #ish to analy9e! aseline cur$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

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