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REFERENCES
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APPENDIX A: Machines used to produce raw toner
Figure A.1: Henschel Mixer (A: Sample container with cooling jacket, B: Power button)
Figure A.2: Extruder
Figure A.3: Crusher
Figure A.4: Jet mill and Classifier
Figure A.5: Blender (A: Sample container, B: timer, C: speed controller)
APPENDIX B: Instruments used for sample characterization
Figure B.1: Mettler Toledo Differential Scanning Calorimeter 822e
Figure B.2: Gel Permeation Chromatography (GPC)
Figure B.3: Ray-ran Melt Flow Indexer (A: specified weight load, B: Automatic Flow Rate
Timer, C: Temperature Controller, D: Heater and Insulation)
Figure B.4: (a) Instrument for tribocharge determination (A: tribometer, B: electrometer, C:
sample cell which held by tribometer)
Figure B.5: Apparatus for Apparent Density Test (A: funnel, B: density cup, C: flowmeter
funnel)
Figure B.6: The Flotest Tester (A: funnel, B: sample container, C: flow disc with holes of
various diameters)
Figure B.7: CILAS 1064 particle size analyzer
Figure B.8: Tectron Ag. 916 Fluxmeter
Figure B.9: QUIKDens 100 Densitometer
APPENDIX C: DSC profiles of toner resins and toners
Figure C.1: DSC profile of L20-TR
Figure C.2: DSC profile of L21-TR
Figure C.3: DSC profile of L22-TR
Figure C.4: DSC profile of L15-TR
Figure C.5: DSC profile of L16-TR
Figure C.6: DSC profile of L23-TR
Figure C.7: DSC profile of L24-TR
Figure C.8: DSC profile of L25-TR
Figure C.9: DSC profile of L18-TR
Figure C.10: DSC profile of H22-TR
Figure C.11: DSC profile of H15-TR
Figure C.12: DSC profile of H16-TR
Figure C.13: DSC profile of H17-TR
Figure C.14: DSC profile of H23-T
Figure C.15: DSC profile of H18-TR
Figure C.16: DSC profile of H19-TR
Figure C.17: DSC profile of M08-TR
Figure C.18: DSC profile of M09-TR
Figure C.19: DSC profile of M10-TR
Figure C.20: DSC profile of M11-TR
Figure C.21: DSC profile of M12-TR
Figure C.22: DSC profile of Commercial Resin A
Figure C.23: DSC profile of Commercial Resin B
Figure C.24: DSC profile of Commercial Resin C
Figure C.25: DSC profile of Commercial Resin D
APPENDIX D: TGA profiles of toners
Figure D.1: TGA curve of M09-FT
Figure D.2: TGA curve of M10-FT
Figure D.3: TGA curve of M11-FT
Figure D.4: TGA curve of magnetite pigment
Figure D.5: TGA curve of charge control agent
APPENDIX E: GPC profiles of toner resins and toners
Figure E.1: GPC profile of L18-TR
Figure E.2: GPC profile of H18-TR
Figure E.3: GPC profile of high molecular weight fraction of M10-TR
Figure E.4: GPC profile of low molecular weight fraction of M10-TR
Figure E.5: GPC profile of high molecular weight fraction of M10-FT
Figure E.6: GPC profile of low molecular weight fraction of M10-FT
APPENDIX F: Particle Size Distribution Data Sheet
Figure F.1: Particle size distribution of M09-FT
Figure F.2: Particle size distribution of M10-FT
Figure F.3: Particle size distribution of M11-FT
APPENDIX G: Calculation of Acid Number of High Molecular Weight Styrene
Acrylic Copolymers and Blended Resins
Standardization of Potassium hydroxide (KOH)
N = (1000 x WKHP) / (204.23 x Veq)
Where, N = Normality of standardized KOH solution
WKHP = Weight of Potassium hydrogen phthalate (KHP) used, g
Veq = Volume of KOH used for the sample titration, ml
204.23 = equivalent weight of KHP
Test 1 Test 2 Test 3
Weight of KHP/ g 0.5068 0.5056 0.5073
Initial reading of KOH, V0 / ml 1.10 0.50 1.00
Final reading of KOH, V1 / ml 32.90 32.50 33.00
Total of KOH used, Veq / ml 31.80 32.00 32.00
Normality, N 0.0780 0.0774 0.0776
Average Normality, N = (NTest 1 + NTest2 + NTest3) / 3
= 0.0777N
Blank Titration of Toluene
Test 1 Test 2 Test 3
Initial reading of KOH, V0 / ml 1.00 1.05 2.00
Final reading of KOH, V1 / ml 1.05 2.00 2.05
Total of KOH used, Vblank / ml 0.05 0.05 0.05
Average Vblank = (Vblank (Test 1) + Vblank (Test 2) + Vblank (Test 3)) / 3
= 0.05ml
Table G.1: Calculation of Acid Number of High Molecular Weight Styrene Acrylic Copolymers
Sample Code H22-TR H15-TR H16-TR H17-TR
Test 1 Test 2 Test 3 Test 1 Test 2 Test 3 Test 1 Test 2 Test 3 Test 1 Test 2 Test 3
Weight of sample/ g 1.0181 1.0405 1.058 1.0103 1.087 1.0455 1.0236 1.0165 1.0155 1.0181 1.021 1.0263
Initial reading of KOH, V0 / ml 1.10 2.20 3.40 4.60 6.55 7.20 8.50 7.80 11.10 1.05 2.10 3.50
Final reading of KOH, V1 / ml 2.20 3.40 4.60 5.75 7.80 8.50 9.55 8.90 12.20 1.95 2.95 4.40
Total of KOH used, Veq / ml 1.10 1.20 1.20 1.15 1.25 1.30 1.05 1.10 1.10 0.90 0.85 0.90
Acid Number / mgKOHg-1 4.50 4.82 4.74 4.75 4.81 5.21 4.26 4.50 4.51 3.64 3.42 3.61
Average 4.68 4.92 4.42 3.55
Sample Code H23-TR H18-TR H19-TR
Test 1 Test 2 Test 3 Test 1 Test 2 Test 3 Test 1 Test 2 Test 3
Weight of sample/ g 1.0372 1.0113 1.0256 1.0435 1.021 1.0115 1.016 1.0359 1.0155
Initial reading of KOH, V0 / ml 3.45 3.60 4.50 1.95 2.95 4.00 2.90 4.80 5.60
Final reading of KOH, V1 / ml 4.20 4.50 5.30 2.90 4.00 5.00 3.45 5.45 6.20
Total of KOH used, Veq / ml 0.75 0.90 0.80 0.95 1.05 1.00 0.55 0.65 0.60
Acid Number / mgKOHg-1 2.94 3.66 3.19 3.76 4.27 4.09 2.15 2.52 2.36
Average 3.26 4.04 2.34
Table G.2: Calculation of Acid Number of Blended Resins
Sample Code M08-TR M09-TR M10-TR
Test 1 Test 2 Test 3 Test 1 Test 2 Test 3 Test 1 Test 2 Test 3
Weight of sample/ g 1.0451 1.0413 1.0495 1.0516 1.0709 1.0402 1.015 1.0137 1.0324
Initial reading of KOH, V0 / ml 4.20 5.00 5.70 4.85 6.00 6.80 5.55 6.30 7.00
Final reading of KOH, V1 / ml 4.85 5.70 6.35 5.55 6.80 7.50 6.30 7.00 7.80
Total of KOH used, Veq / ml 0.65 0.70 0.65 0.70 0.80 0.70 0.75 0.70 0.80
Acid Number / mgKOHg-1 2.50 2.72 2.49 2.69 3.05 2.72 3.01 2.80 3.17
Average 2.57 2.82 2.99
Sample Code M11-TR M12-TR
Test 1 Test 2 Test 3 Test 1 Test 2 Test 3
Weight of sample/ g 1.039 1.1827 1.0261 1.0039 1.0132 1.0226
Initial reading of KOH, V0 / ml 6.30 7.50 8.40 7.10 4.00 4.80
Final reading of KOH, V1 / ml 7.10 8.40 9.20 7.85 4.80 5.65
Total of KOH used, Veq / ml 0.80 0.90 0.80 0.75 0.80 0.85
Acid Number / mgKOHg-1 3.15 3.13 3.19 3.04 3.23 3.41
Average 3.16 3.23
APPENDIX H: Calculation of Percentage of THF Insoluble Fraction of High Molecular Weight Styrene Acrylic Copolymers and
Blended Resins
Table H.1: Calculation of Percentage of THF Insoluble Fraction of High Molecular Weight Styrene Acrylic Copolymers
Sample Code H22-TR H15-TR H16-TR H17-TR H23-TR H18-TR H19-TR
Weight of sample, w/ g 1.0413 1.0324 1.1827 1.0137 1.1495 1.0261 1.0644
Weight of filter paper, w0/ g 0.7935 0.7965 0.8032 0.7806 0.7824 0.7948 0.7985
Weight of (filter paper + residue), w1/ g 0.8989 0.9244 1.0245 0.9170 0.8888 0.9677 1.5215
w1-w0 /g 0.1054 0.1279 0.2213 0.1364 0.1064 0.1729 0.7230
% THF Insoluble Fraction 10.12 12.39 18.71 13.46 9.26 16.85 67.93
Table H.2: Calculation of Percentage of THF Insoluble Fraction of Blended Resins
Sample Code M08-TR M09-TR M10-TR M11-TR M12-TR
Weight of sample, w/ g 1.0402 1.0145 1.0338 1.0048 1.0108
Weight of filter paper, w0/ g 0.7986 0.7910 0.7909 0.7909 0.7971
Weight of (filter paper + residue), w1/ g 0.8918 0.8862 0.8879 0.9294 0.9324
w1-w0 /g 0.0932 0.0952 0.0970 0.1385 0.1353
% THF Insoluble Fraction 8.96 9.38 9.38 13.78 13.39
APPENDIX I: Estimation of Tg by using Fox equation and Gordon-Taylor equation
(a) Fox equation:
Where Tg1 = Tg‘s of the poly(butyl acrylate), 218 K
Tg2 = Tg‘s of the polystyrene, 373 K
w1 = respective weight fractions of poly(butyl acrylate) in the mixture
w2 = respective weight fractions of polystyrene in the mixture.
Example:
Sample L20-TR, w1 = 0.25 and w2 = 0.75
Where Tg1 = 218 K and Tg2 = 373 K
So, Tg = 316.70 K
Likewise, Tg of other samples were calculated.
Table I.1: Estimation of Tg of Low Molecular Weight Styrene Acrylic Copolymers by
using Fox equation
Sample L20-TR L21-TR L22-TR L15-TR L-16TR
Tg /K 316.70 326.56 337.05 348.24 360.19
Table I.2: Estimation of Tg of High Molecular Weight Styrene Acrylic Copolymers by
using Fox equation
Sample H22-TR H15-TR H16-TR H17-TR H23-TR
Tg /K 316.35 326.18 336.65 347.81 359.73
(b) Gordon-Taylor equation:
Where Tg1 = Tg‘s of the poly(butyl acrylate), 218 K
Tg2 = Tg‘s of the polystyrene, 373 K
w1 = respective weight fractions of poly(butyl acrylate) in the mixture
w2 = respective weight fractions of polystyrene in the mixture.
k = fitting factor
Calculation of k
Example:
Sample L20-TR, w1 = 0.25 and w2 = 0.75
Where Tg1 = 218 K, Tg2 = 373 K and Tg = Tg exp = 312 K
So, k = 0.5137
Likewise, k of other samples was calculated.
Table I.3: Calculation of fitting factor, k of Low Molecular Weight Styrene Acrylic
Copolymers by using Gordon-Taylor equation
Sample L20-TR L21-TR L22-TR L15-TR L-16TR
k 0.5137 0.4298 0.3396 0.2716 0.1679
Average k = 0.3445
Table I.4: Calculation of fitting factor, k of High Molecular Weight Styrene Acrylic
Copolymers by using Gordon-Taylor equation
Sample H22-TR H15-TR H16-TR H17-TR H23-TR
k 0.7273 0.7273 0.5860 0.5056 0.3556
Average k = 0.5804
Calculation of Tg
(i) Low Molecular Weight Styrene Acrylic Copolymers
Tg of other samples was calculated by fitting k = 0.3445 into the Gordon-Taylor equation.
Example:
Sample L20-TR, w1 = 0.25 and w2 = 0.75
Where Tg1 = 218 K, Tg2 = 373 K, and k = 0.3445,
So, Tg = 296.78 K
Likewise, Tg of other samples were calculated.
Table I.5: Estimation of Tg of Low Molecular Weight Styrene Acrylic Copolymers by
using Gordon-Taylor equation
Sample L20-TR L21-TR L22-TR L15-TR L-16TR
Tg /K 296.78 307.82 320.68 335.20 352.46
(ii) High Molecular Weight Styrene Acrylic Copolymers
Tg of other samples was calculated by fitting k = 0.5804 into the Gordon-Taylor equation.
Example:
Sample H20-TR, w1 = 0.28 and w2 = 0.70
Where Tg1 = 218 K, Tg2 = 373 K, and k = 0.5804,
So, Tg = 309.76 K
Likewise, Tg of other samples were calculated.
Table I.6: Estimation of Tg of High Molecular Weight Styrene Acrylic Copolymers by
using Gordon-Taylor equation
Sample H22-TR H15-TR H16-TR H17-TR H23-TR
Tg /K 309.76 319.42 329.70 340.67 352.41
APPENDIX J
Test Print Images of M09-FT
APPENDIX K
Test Print Images of M10-FT
APPENDIX L
Test Print Images of M11-FT
APPENDIX M
Test Print Images of commercial toner A