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- ぜんぺい みうら
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1 Graduate School of Education, Hiroshima University 1
2 1. 2. TG, TG-DTA TG 5. TG-DTA 6. TG 7. TG 8. TG 9. TG-DTA-EGA 2
3 3
4 (Thermogravimetry) TG (Derivative TG) DTG (Evolved Gas Detection) EGD (Evolved Gas Analysis) (Emanation Thermal Analysis) EGA ETA (Differential Thermal Analysis) DTA H (Differential Scanning Calorimetry) DSC (Thermodilatometry) (Thermomechanical Analysis) TMA (Dynamic Thermomechanometry) DMA (Thermosonimetry) (Thermoacoustimetry) (Thermoelectrometry) (Thermomagnetmetry) 4
5 1. TG 1.1 TG 5
6 1.2 (1) TG N S 6
7 1.2 (2) (a) Suspending (b) Top-loading (c) Horizontal 7
8 1.2 (3) 8
9 1.2 (4) R S C A A C T T 9
10 1.3 (1) TG N S 1
11 (1) (2) CaC 2 O 4 H 2 O (1) CaC 2 O 4 H 2 O CaC 2 O 4 +H 2 O (2) CaC 2 O 4 CaCO 3 +CO 2 (3) CaCO 3 CaO+CO 2 Mass change / mg H 2 O (-12.3%) -CO (-19.2%) -CO 2 (-3.1%) Temperature / C 11
12 2.2 (1) (1) N S (a) Experimental arrangement Apparent mass A: Permanorm B: Ni C: Mumetal D: Permanorm 5 E: Trafoperm T / C (b) TG curve for GM761 12
13 2.2 (2) (2) Zn ( ) In Sn Pb Zn Al
14 2.2 (3) m / mg DTA TG DTG (d m/dt) / mg min DTA / µv T / C -5 Pb(1.29mg), Zn(6.63mg), Ni(54.99mg) 14
15 3. TG 3.1 (1) (2) (3) (4) (6) (5) 15
16 3.1 Isothermal Measurement T / K (1) Isothermal W (d W/dt) T W / mg (d W/dt) / mg min t / min CuCO 3 Cu(OH) 2 2CuO + CO 2 + H 2 O 16
17 3.1 17
18 3.1 Nonisothermal Measurement T / K (2) Nonisothermal W T (d W/dt) W / mg (d W/dt) / mg min t / min CuCO 3 Cu(OH) 2 2CuO + CO 2 + H 2 O 18
19 3.1 (1) CuSO 4 5H 2 O CuSO 4 3H 2 O + 2H 2 O (2) CuSO 4 3H 2 O CuSO 4 H 2 O + 2H 2 O (3) CuSO 4 H 2 O CuSO 4 + H 2 O 19
20 3.1 (Self-cooling Effect) (1) CaC 2 O 4 H 2 O CaC 2 O 4 +H 2 O (2) CaC 2 O 4 CaCO 3 +CO 2 (3) CaCO 3 CaO+CO 2 DTA 2
21 3.1 Li 2 SO 4 H 2 O Li 2 SO 4 + H 2 O 21
22 3.1 Controlled Rate Measurement T / K (3) Constant Rate W T (d W/dt) W / mg (d W/dt) / mg min -1 t / min CuCO 3 Cu(OH) 2 2CuO + CO 2 + H 2 O 22
23 3.2 (1) 23
24 3.2 (2) TG-DTA 24
25 3.2 (3) 1. Fractional reaction α Time / min mg 5. mg 1. mg 2. mg Li 2 SO 4 H 2 O Li 2 SO 4 + H 2 O
26 3.3 (1) (2) B A D (3) C 26
27 3.3 27
28 4 TG-DTA TG DTA TG DTA 28
29 4 TG-DTA TG-DTA 12 1 T / K DTA TG Weight change W / mg δ T / µv Time / min 29
30 5. TG 5.1 Mass change / x1-3 mg (a) (b) Mass change / mg Temperature / C TG 3
31 5.2 (mg) (%) 1 (mg) Mass change / mg H 2 O (-12.3%) -CO (-19.2%) -CO 2 (-3.1%) Temperature / C 31
32 5.3 TG (dm/dt) (dm/dt) (DTG) vs. T.5. T e.o dm/dt / mg min T o T o : T e.o. : T p Temperature / C T p : 32
33 5.4 α = m m m m f m : m f : m: Fractional reaction α Temperature / C (dα/dt) / x1-3 s -1 33
34 6. TG 6.1 (CRTA) (a) (b) CRTA Chronometer Programmer Chronometer Programmer X-meter Thermometer X-meter Thermometer Recorder Controller Recorder Controller 34
35 6.1 CRTG B A TG circuit DTG circuit CRTA Prog. Temp. Prog. Recorder Chronometer C Regulator Thermometer CRTA Controller 35
36 6.2 CRTG T / K (3) Constant Rate W T (d W/dt) t / min W / mg CuCO 3 Cu(OH) 2 2CuO + CO 2 + H 2 O (d W/dt) / mg min -1 36
37 6.3 CRTG 11.6 T / K 1 W -4 9 T (d W/dt) Time / min Mass change W / mg (d W/dt) / mg min -1 CaCO3 CaO + CO 2 37
38 6.4 CRTG 38
39 7. TG 39
40 7.1 TG(/DTA)-FTIR 4
41 7.2 TG(/DTA)-MS 41
42 7.3 TG(/DTA)-GC-MS 42
43 7.4 TG-FTIR TG-MS TG-FTIR TG-MS He, Air, N 2 43
44 7.5 TG-MS (a) m / mg (b) I / x1-9 A (c) I / x1-9 A DTA TG TIC m/z=18 m/z=28 m/z= T / C m/z DTA / µv (1) CaC 2 O 4 H 2 O CaC 2 O 4 +H 2 O (2) CaC 2 O 4 CaCO 3 +CO 2 (3) CaCO 3 CaO+CO 2 44
45 7.6 CREGA-TG 45
46 7.7 CREGA-TG m / mg (a) TG H 2 O CO 2 DTA / g m -3 DTA / µv T / K (b) T CO 2 TG / g m -3 m / mg T / K time / min CuCO 3 Cu(OH) 2 2CuO + CO 2 + H 2 O 46
CuSO POINT S 2 Ni Sn Hg Cu Ag Zn 2 Cu Cu Cu OH 2 Cu NH CuSO 4 5H 2O Ag Ag 2O Ag 2CrO4 Zn ZnS ZnO 2+ Fe Fe OH 2 Fe 3+ Fe OH 3 2 Cu Cu OH 2 Ag Ag
CuSO POINT S 2 Ni Sn Hg Cu Ag Zn 2 CuCu Cu OH 2 Cu NH 3 4 2 CuSO 4 5H 2O AgAg 2O Ag 2CrO4 ZnZnS ZnO 2+ Fe Fe OH 2 Fe 3+ Fe OH 3 2 Cu Cu OH 2 Ag Ag 2O Cl Cl AgCl PbCl 2 Ag Cl AgCl Pb 2 2Cl PbCl2 Cl Hg22
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X線分析の進歩36 別刷
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