BiofuelsGS 2 Analytical techniques in combustion Part 4, ÅA. TGA DTA Group 4 Norazana, Daniel, Johan
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1 BiofuelsGS 2 Analytical techniques in combustion Part 4, ÅA TGA DTA Group 4 Norazana, Daniel, Johan
2 Presentation outline Comparison of DTA and TGA techniques Group works G1. Indium (DTA) G3. Oxalate (TGA) Method approval G2. KCl (TGA DTA) G5. K2SO4 (TGA DTA) G4. KCl K2SO4 eut mix (TGA DTA) Phase diagram
3 DTA TGA one instrument two functions DTA Temperature difference Thermocouple Structural changes Chrystallization Melting Chemical reactions causing temperature changes TGA Mass change Microbalance Mass change by phase transition Vaporization Sublimation Mass change by chemical reactions
4 Indium Standard for DTA ^exo Experiment: In-Al _LF, :10:35 SDTA In-Al _LF, :29 In-Al _LF, mg Method Name: Blank In-Al _LF Method: Blank In-Al _LF /min N ml/min ^exo 0.0 []SDTA In-Al _LF, : In-Al _LF, mg Integral s normalized ksg^-1 Onset Heating Rate min^-1 Result Mode Sample Temp Melting point: Litterature: 156,6 Experimental: 153,95 min min
5 Calcium oxalate, CaC 2 O 4 H2O Common material to show the TGA performance Step 1: release of water Step 2: release of CO Step 3: release of CO 2 -H 2 O % Experiment: oxalate group 3, :36:40!oxalate group 3 oxalate g roup 3, mg 100 Method Name: Blank, no Lid, Oxalate 90 Module: TGA/SDTA851e/LF1600/UMT5/552, :28: CO CO min
6 KCl K 2 SO 4 experiments In these experiments the 2 pure salts and an eutectic mixture were analyzed by DTA TGA The results were compared with theoretical values In order to create a complete phase diagram of a salt mixture the melting behavior of the pure salts and several mixtures are needed.
7 Method KCl Pure KCl KCl K 2 SO 4 eutectic mixture TG KCl blank _LF :39: N2 50 ml/min Expected Mp(KCl): 771 Mp(Eut.): 690 Temp prog. Start T: 25 End T: 830 Heating rate: 20 /min Gas: N 2 Flow rate: 50 ml / min min e STAR SW 8.10
8 Pure KCl ^exo Melting point: Litterature: 771 Experimental: 770,29 ^exo []SDTA KCl_100%_g roup2, :52: KCl_100%_g roup2, mg SDTA KCl_100%_group2, :52:35 KCl_100%_g roup2, mg Integral s normalized ksg^-1 Onset Heating Rate min^-1 Result Mode Sample Temp min min
9 Pure K 2 SO 4 Phase transition: Litterature: 587 ^exo Melting point: Litterature: Method: Blank + Lid_K2SO4 100%_ _LF /min N ml/min SDTA!K2SO4 100%_ _Group 5, K2SO4 100%_ _Group 5, mg Experiment: K2SO4 100%_ _Group 5, :49:24 Correct Baseline????? min
10 Phase transition and melting Experimental ^exo 582, ,94 ^exo []SDTA! K2SO4 100%_ _Group 5, K2SO4 100%_ _Group 5, mg Integral s normalized ksg^-1 Onset Heating Rate min^-1 Result Mode Sample Temp -1.0 Integral s normalized ksg^-1 Onset Heating Rate min^-1 Result Mode Sample Temp min min
11 Sample preparation KCl K 2 SO 4 eutectic mixture 26 mole % K 2 SO 4 74 mole % KCl 45 mg K 2 SO 4 55 mg KCl
12 TGA curve KCl K 2 SO 4 eutectic mixture %!KCL-K2SO4 eut.mixt _Group 4 KCL-K2SO4 eut.mixt _Group 4, mg min STAR e SW 8.10
13 SDTA curve kg^-1 KCl K 2 SO 4 eutectic mixture Experiment: KCL-K2SO4 eut.mixt _Group 4, :09:58!SDTA KCL-K2SO4 eut.mixt _Group KCL-K2SO4 eut.mixt _Group 4, mg Method Name: KCl blank _LF Integral s normalized ksg^-1 Onset Heating Rate m in^-1 Result Mode Sample Temp Integral s normalized ks g^-1 Onset Heating Rate m in^-1 Result Mode Sample Tem p min
14 Phase transformation peak KCl K 2 SO 4 eutectic mixture ^exo Integral s normalized ksg^-1 Onset Heating Rate min^-1 Result Mode Sample Temp Phase Transformation min
15 Melting peak KCl K 2 SO 4 eutectic mixture kg^ Integral s normalized ks g^-1 Onset Heating Rate m in^-1 Result Mode Sample Temp Mp min
16 ^exo % TGA DTA KCl K 2 SO 4 eutectic mixture TGA DTA min min
17 Summary [] KCl Eut. Mix. K 2 SO 4 PT theory PT exp. 580,08 582,54 MP theory MP exp. 770,29 683, ,94 PT = phase transition MP = melting point
18 Conclusions KCl and K 2 SO 4 system: DTA results are in good agreement with the theoretical phase diagram Depending on fuel mixtures the melting range of the possibly forming salts have to be taken into careful consideration
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