Anlisis Cuantitativo (TOPAS)

Despus del anlisis cualitativo donde se determinaron las fases que contena la muestra, se cargaron estas en el TOPAS para su posterior tratamiento.

Posteriormente se refinaron las constantes de celda y el tamao del cristalito para cada una de las fases presentes.

Una vez refinadas las constantes de celda y tamao del cristalito de procedi a refinar las posiciones de cada uno de los tomos presentes en la fases de la muestra.

Se le dio la orientacin preferencial para la fase de Kaolinita A con un hkl de ( 0 0 1)

Anlisis cuantitativo sin ingresar el valor del corindn

Comparando los valores que tenemos del cuantitativo del corindn (19.98) con el valor que obtenemos haciendo el tratamiento, podemos observar que este es un poco alejado del deseado pero despus del refinamiento es el que nos arroja un residual ms bajo. Despus de probar con varios .cif para el cuarzo llegamos a la conclusin que el que mejor se ajusta fue el que empleamos (poner el serial ese para identificar ese cuarzo).

Al ingresar los valores de hkl en la orientacin preferencial para kaolinita (0 0 1) y para cuarzo (1 0 1 ), se observ un aumento en el porcentaje de amorfo del material pero una notable disminucin en el valor de rpw pasando de un 11 aproximadamente, a un 9

A continuacin se adjunta el .tex con los parmetros trabajados para la muestra c8vy.raw, donde se encontr como fases el corindn (19.98%), cuarzo(10.364), gibbsita(11.923) y kaolinita(23.503) y un contenido amorfo de (34.32%).

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R-Values

Rexp : 2.90 Rwp : 9.08 Rp : 5.99 GOF : 3.13Rexp`: 10.18 Rwp`: 31.85 Rp` : 30.37 DW : 0.33

Quantitative Analysis, Wt% Rietveld Spiked Original Amorphous content 0 34.320 42.8411 *Corundum 30.283 19.890 0.0002 Quartz 15.779 10.364 12.9373 Gibbsite 18.154 11.923 14.8844 "Kaolinite 1A" 35.784 23.503 29.338

Background Chebychev polynomial, Coefficient 0 1156.232 1 -890.2926 2 624.1541 3 -381.8915 4 195.8922 5 -111.1875

Instrument Primary radius (mm) 280 Secondary radius (mm) 280 Linear PSD 2Th angular range () 2.93 FDS angle () 0.6 Full Axial Convolution Filament length (mm) 12 Sample length (mm) 15 Receiving Slit length (mm) 12 Primary Sollers () 2.5 Secondary Sollers () 2.5

Corrections Zero error 0.03259788 LP Factor 90

Miscellaneous Start X 8

Structure 1 Phase name Corundum R-Bragg 99.846 Spacegroup R-3cH Scale 0.00123276315 Cell Mass 611.768 Cell Volume (^3) 255.08619 Wt% - Rietveld 30.283 Wt% in Spiked sample 19.890 Wt% in Original sample 0.000 Crystallite Size Cry size Lorentzian (nm) 223.5 Crystal Linear Absorption Coeff. (1/cm) 126.415 Crystal Density (g/cm^3) 3.982 Lattice parameters a () 4.7600080 c () 12.9999281

Site Np x y z Atom Occ Beq Al1 12 0.00000 0.00000 0.39427 Al+3 1 13.74O1 18 0.36805 0.00000 0.25000 O-2 1 14.84

Structure 2 Phase name Quartz R-Bragg 99.865 Spacegroup P3221 Scale 0.00335100616 Cell Mass 264.508 Cell Volume (^3) 113.08720 Wt% - Rietveld 15.779 Wt% in Spiked sample 10.364 Wt% in Original sample 12.937 Crystallite Size Cry size Lorentzian (nm) 255.4 Crystal Linear Absorption Coeff. (1/cm) 174.424 Crystal Density (g/cm^3) 3.884 Preferred Orientation (Dir 1 : 0 1 0) 1.2131 Lattice parameters a () 4.9153179 c () 5.4047998

Site Np x y z Atom Occ Beq Si 6 0.46266 0.00000 0.00000 Si+4 1 1O 6 0.37873 0.20130 0.14532 O-2 1 1

Structure 3 Phase name Gibbsite R-Bragg 99.745 Spacegroup P121/n1 Scale 0.000448331271 Cell Mass 599.837 Cell Volume (^3) 428.82879 Wt% - Rietveld 18.154 Wt% in Spiked sample 11.923 Wt% in Original sample 14.884 Crystallite Size Cry size Lorentzian (nm) 448.7 Crystal Linear Absorption Coeff. (1/cm) 58.677 Crystal Density (g/cm^3) 2.323 Lattice parameters a () 8.5442301 b () 5.1794295 c () 9.7270434 beta () 94.99398

Site Np x y z Atom Occ Beq O1 4 0.18354 0.45604 -0.15287 O-2 1 1O2 4 0.65893 0.82063 -0.13521 O-2 1 1O3 4 0.14887 0.13747 -0.06934 O-2 1 1O4 4 0.02503 0.36401 -0.21401 O-2 1 1O5 4 0.18298 0.74353 -0.06470 O-2 1 1O6 4 0.61658 0.14305 -0.16077 O-2 1 1Al1 4 0.32949 0.50000 0.00000 Al+3 1 1Al2 4 0.25206 0.00000 0.00000 Al+3 1 1

Structure 4 Phase name Kaolinite 1A R-Bragg 99.868 Spacegroup C1 Scale 0.00134743198 Cell Mass 508.256 Cell Volume (^3) 331.93123 Wt% - Rietveld 35.784 Wt% in Spiked sample 23.503 Wt% in Original sample 29.338 Crystallite Size Cry size Lorentzian (nm) 15.0 Crystal Linear Absorption Coeff. (1/cm) 79.360 Crystal Density (g/cm^3) 2.543 Preferred Orientation (Dir 1 : 0 0 1) 0.7866939 Lattice parameters a () 5.2357211 b () 8.8832498 c () 7.4305364 alpha () 92.84378 beta () 105.9156 gamma () 89.59145

Site Np x y z Atom Occ Beq O1 2 0.42716 0.13962 -0.11625 O-2 1 0.4737O2 2 0.30526 0.22721 -0.30997 O-2 1 0.4737O3 2 0.13694 0.09352 -0.03752 O-2 1 0.4737O4 2 0.06665 0.34315 -0.05546 O-2 1 0.4737O5 2 0.80494 0.30466 0.11174 O-2 1 0.4737O6 2 0.30520 -0.19520 0.11210 O-2 1 0.4737O7 2 1.07411 0.19027 0.59110 O-2 1 0.4737O8 2 0.68097 -0.56071 0.39027 O-2 1 0.4737O9 2 -0.27498 0.16715 0.70551 O-2 1 0.4737Al1 2 0.63426 0.06576 0.08594 Al+3 1 0.8685Al2 2 -0.03472 0.41023 -0.00772 Al+3 1 0.8685Si1 2 1.00749 0.28074 0.44478 Si+4 1 0.7106Si2 2 0.86173 0.06038 0.43742 Si+4 1 0.7106

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R-Values

Rexp : 2.63 Rwp : 9.80 Rp : 6.27 GOF : 3.72Rexp`: 9.77 Rwp`: 36.34 Rp` : 33.99 DW : 0.20

Quantitative Analysis - Rietveld Phase 1 : Corundum 27.263 % Phase 2 : Quartz 13.756 % Phase 3 : Gibbsite 8.752 % Phase 4 : "Kaolinite 1A" 50.229 %

Background Chebychev polynomial, Coefficient 0 1646.818 1 -1816.828 2 1333.334 3 -820.2034 4 431.054 5 -204.6924

Instrument Primary radius (mm) 280 Secondary radius (mm) 280 Linear PSD 2Th angular range () 2.93 FDS angle () 0.6 Full Axial Convolution Filament length (mm) 12 Sample length (mm) 15 Receiving Slit length (mm) 12 Primary Sollers () 2.5 Secondary Sollers () 2.5

Corrections Zero error 0.02892148 LP Factor 90

Structure 1 Phase name Corundum R-Bragg 13.370 Spacegroup R-3cH Scale 0.00123585819 Cell Mass 611.768 Cell Volume (^3) 255.00431 Wt% - Rietveld 27.263 Crystallite Size Cry size Lorentzian (nm) 250.8 Crystal Linear Absorption Coeff. (1/cm) 126.456 Crystal Density (g/cm^3) 3.984 Lattice parameters a () 4.7595731 c () 12.9981304

Site Np x y z Atom Occ Beq Al1 12 0.00000 0.00000 0.39394 Al+3 1 13.74O1 18 0.36288 0.00000 0.25000 O-2 1 14.84

Structure 2 Phase name Quartz R-Bragg 7.385 Spacegroup P3221 Scale 0.0032526612 Cell Mass 264.508 Cell Volume (^3) 113.07218 Wt% - Rietveld 13.756 Crystallite Size Cry size Lorentzian (nm) 217.0 Crystal Linear Absorption Coeff. (1/cm) 174.447 Crystal Density (g/cm^3) 3.884 Preferred Orientation (Dir 1 : 0 1 0) 1.923317 Lattice parameters a () 4.9150325 c () 5.4047094

Site Np x y z Atom Occ Beq Si 6 0.48493 0.00000 0.00000 Si+4 1 1O 6 0.41491 0.25858 0.15175 O-2 1 1

Structure 3 Phase name Gibbsite R-Bragg 7.211 Spacegroup P121/n1 Scale 0.00024040822 Cell Mass 599.837 Cell Volume (^3) 429.21294 Wt% - Rietveld 8.752 Crystallite Size Cry size Lorentzian (nm) 537.6 Crystal Linear Absorption Coeff. (1/cm) 58.624 Crystal Density (g/cm^3) 2.321 Preferred Orientation (Dir 1 : 2 0 -2) 0.5870895 Lattice parameters a () 8.5426925 b () 5.1858702 c () 9.7251347 beta () 94.97501

Site Np x y z Atom Occ Beq O1 4 0.21109 0.39904 -0.17452 O-2 1 1O2 4 0.69802 0.73556 -0.10856 O-2 1 1O3 4 0.16742 0.13382 -0.06680 O-2 1 1O4 4 0.07491 0.44645 -0.15308 O-2 1 1O5 4 0.12731 0.73652 -0.07407 O-2 1 1O6 4 0.63792 0.09289 -0.14311 O-2 1 1Al1 4 0.32009 0.50000 0.00000 Al+3 1 1Al2 4 0.26410 0.00000 0.00000 Al+3 1 1

Structure 4 Phase name Kaolinite 1A R-Bragg 6.814 Spacegroup C1 Scale 0.00207858322 Cell Mass 508.256 Cell Volume (^3) 336.23052 Wt% - Rietveld 50.229 Crystallite Size Cry size Lorentzian (nm) 13.2 Crystal Linear Absorption Coeff. (1/cm) 78.345 Crystal Density (g/cm^3) 2.510 Preferred Orientation (Dir 1 : 0 0 1) 0.8376787 Lattice parameters a () 5.3305691 b () 8.8691292 c () 7.4097566 alpha () 93.16941 beta () 105.993 gamma () 88.69539

Site Np x y z Atom Occ Beq O1 2 0.39236 0.11803 -0.07559 O-2 1 0.4737O2 2 0.32618 0.26235 -0.23563 O-2 1 0.4737O3 2 -0.02395 0.08492 0.04583 O-2 1 0.4737O4 2 0.13204 0.34526 0.04970 O-2 1 0.4737O5 2 0.67900 0.26939 0.11904 O-2 1 0.4737O6 2 0.37324 -0.15823 0.18156 O-2 1 0.4737O7 2 1.23858 0.15516 0.62777 O-2 1 0.4737O8 2 0.73343 -0.51609 0.41574 O-2 1 0.4737O9 2 -0.27360 0.15349 0.74950 O-2 1 0.4737Al1 2 0.72877 0.08015 0.20299 Al+3 1 0.8685Al2 2 -0.08482 0.49311 0.05707 Al+3 1 0.8685Si1 2 0.92578 0.27069 0.52818 Si+4 1 0.7106Si2 2 0.91712 0.05225 0.48906 Si+4 1 0.7106