Hello everyone,
I tried to apply Martin Fisch's K factor macros on CPD-3 data but have some problems; could you please help me to fix it? where did I go wrong? how should we enter the XRF results?
Thank you very much!
Kind regards,
Eric
here is my INP file:
o_errors
'--------------------------------------------------------'
' K Factor calculation from external standard starts here
' OConnor & Raven, Powder Diffraction 3(1) (1988) 2-6
'--------------------------------------------------------'
xdd "C:\TOPAS5\Tutorial\Quantitative phase analysis\External Standard Method\CORUNDUM.RAW" 'XRD Pattern of external standard'
'rebin_with_dx_of 0.02
r_wp 0 r_exp 0 r_p 0 gof 0
bkg @ 0 0 0 0 0 0
Specimen_Displacement(SD_Corundum, 0)
start_X 20
str 'Többens, D.M. et al., Mat. Sci. Forum 378 (2001) 288-293'
phase_name "Corundum"
a a_Corundum 4.76 min 4.74 max 4.78
b = Get(a);
c c_Corundum 12.99 min 12.9 max 13.1
ga 120
space_group 167
site Al1 x =0; y =0; z 0.3522 occ AL+3 1 beq 0.30
site O1 x 0.6937 y =0; z =1/4; occ O-2 1 beq 0.33
scale Scale_Corundum 0.00001
CS_L(CSL_Corundum, 400 min 50 max 5000)
Strain_L(StrainL_Corundum, 0.01 min 0.001 max 1)
cell_volume Volume_Corundum 0
cell_mass Mass_Corundum 0
phase_MAC MAC_Corundum 0
weight_percent WP_Corundum 0
prm !Crystallinity_Corundum 98
prm Corundum_Lac = Get(mixture_MAC) Get(mixture_density_g_on_cm3);: 0
'Calculation of K-Factor from external standard'
prm !KFactor = Scale_Corundum * ( 1.660538921 * (Mass_Corundum/Volume_Corundum) ) * Volume_Corundum2 * MAC_Corundum / (Crystallinity_Corundum) ;: 0
'Macro for wt.-% from scale, MAC, cell volume and KFactor'
macro wt_percent_K_MAC(result) { prm = ( ( Get(scale) * ( 1.660538921 * (Get(cell_mass)/Get(cell_volume)) ) * (Get(cell_volume))2) * MAC_Sample ) / KFactor ;: result }
'Dummy phases are used for energy dependent oxide MAC calculation'
macro d_str { dummy_str space_group P1 scale 0 a 1 b 1 c 1 site }
d_str Si occ Si+4 = 1; site O occ O-2 = 2; prm MAC_SiO2 = Get(phase_MAC); : 35.81264
d_str Al occ Al+3 = 2; site O occ O-2 = 3; prm MAC_Al2O3 = Get(phase_MAC); : 31.59020
d_str Fe occ Fe+3 = 2; site O occ O-2 = 3; prm MAC_Fe2O3 = Get(phase_MAC); : 214.26272
d_str Ca occ Ca+2 = 1; site O occ O-2 = 1; prm MAC_CaO = Get(phase_MAC); : 124.46608
d_str Zn occ Zn+2 = 1; site O occ O-2 = 1; prm MAC_ZnO = Get(phase_MAC); : 48.611
d_str F occ F-1 = 2; site Ca occ Ca+2 = 1; prm MAC_CaF2 = Get(phase_MAC); : 94.718
d_str Mg occ Mg+2 = 1; site O occ O-2 = 1; prm MAC_MgO = Get(phase_MAC); : 28.61699
d_str S occ S = 1; site O occ O-2 = 3; prm MAC_SO3 = Get(phase_MAC); : 44.15801
d_str K occ K+1 = 2; site O occ O-2 = 1; prm MAC_K2O = Get(phase_MAC); : 122.06126
d_str Na occ Na+1 = 2; site O occ O-2 = 1; prm MAC_Na2O = Get(phase_MAC); : 24.93736
d_str Ti occ Ti+4 = 1; site O occ O-2 = 2; prm MAC_TiO2 = Get(phase_MAC); : 124.23941
d_str Sr occ Sr+2 = 1; site O occ O-2 = 1; prm MAC_SrO = Get(phase_MAC); : 97.04589
d_str P occ P = 2; site O occ O-2 = 5; prm MAC_P2O5 = Get(phase_MAC); : 39.33911
d_str Mn occ Mn+3 = 2; site O occ O-2 = 3; prm MAC_Mn2O3 = Get(phase_MAC); : 191.01235
d_str Cr occ Cr+3 = 2; site O occ O-2 = 3; prm MAC_Cr2O3 = Get(phase_MAC); : 172.14416
d_str C occ C = 1; site B occ O-2 = 2; prm MAC_LOI_CO2 = Get(phase_MAC); : 9.57292
d_str H occ H = 2; site O occ O-2 = 1; prm MAC_LOI_H2O = Get(phase_MAC); : 10.23680
d_str La occ La+3 = 1; site B occ B = 6; prm MAC_LaB6 = Get(phase_MAC); : 237.33852
d_str Zr occ Zr+4 = 1; site Si occ Si+4 = 1; site O occ O-2 = 4; prm MAC_ZrSiO4 = Get(phase_MAC); : 83.19554
'-----------------------------------------------------------------------------'
' Part for phase quantification in sample using external standard starts here'
'-----------------------------------------------------------------------------'
xdd "C:\TOPAS5\Tutorial\Quantitative phase analysis\External Standard Method\CPD-3.raw" 'XRD Pattern of sample'
'rebin_with_dx_of 0.02
r_wp 0 r_exp 0 r_p 0 gof 0
bkg @ 0 0 0 0 0 0
Specimen_Displacement(@, 0)
'XRF wt.-% data of sample (change prm_with_error to prm for version 5)'
prm !SiO2 27.77_0
prm !Al2O3 31.78_0
prm !Fe2O3 0_0
prm !CaO 0_0
prm !ZnO 20.10_0
prm !CaF2 20.35_0
prm !MgO 0_0
prm !SO3 0_0
prm !K2O 0_0
prm !Na2O 0_0
prm !TiO2 0_0
prm !SrO 0_0
prm !P2O5 0_0
prm !Mn2O3 0_0
prm !Cr2O3 0_0
prm !ZrSiO4 0_0
prm !LaB6 0_0
prm !LOI_CO2 0_0 'Loss on ignition'
prm !LOI_H2O 0_0 'Loss on ignition'
'MAC calculation from XRF data'
prm !MAC_Sample =
SiO20.01MAC_SiO2 + Al2O30.01MAC_Al2O3 + CaF20.01MAC_CaF2 +
Fe2O30.01MAC_Fe2O3 + CaO0.01MAC_CaO + ZnO0.01MAC_ZnO +
MgO0.01MAC_MgO + SO30.01MAC_SO3 + K2O0.01MAC_K2O +
Na2O0.01MAC_Na2O + TiO20.01MAC_TiO2 + SrO0.01MAC_SrO +
P2O50.01MAC_P2O5 + Mn2O30.01MAC_Mn2O3 + Cr2O30.01MAC_Cr2O3 +
ZrSiO40.01MAC_ZrSiO4 + LaB60.01MAC_LaB6 + LOI_CO20.01MAC_LOI_CO2 +
LOI_H2O0.01MAC_LOI_H2O;: 0
str
LVol_FWHM_CS_G_L( 1, 0, 0.89, 0,,,@, 1000)
e0_from_Strain( 0,,,@, 0.1)
r_bragg 0
phase_MAC 0
phase_name "Fluorite"
MVW( 0, 0, 0)
corrected_weight_percent 0
space_group F_M_-3_M
scale @ 0.0001
K_Factor_WP( 0)
Phase_LAC_1_on_cm( 0)
Phase_Density_g_on_cm3( 0)
Cubic(@ 5.46379)
site Ca num_posns 0 x 0 y 0 z 0 occ Ca 1 beq 0.4856
site F num_posns 0 x 0.25 y 0.25 z 0.25 occ F 1 beq 0.72
Preferred_Orientation(@, 1_LIMIT_MAX_1 min =0; max =1;,, 1 1 1)
str
LVol_FWHM_CS_G_L( 1, 0, 0.89, 0,,,@, 1000)
e0_from_Strain( 0,,,@, 0.1_LIMIT_MIN_0.0001)
r_bragg 0
phase_MAC 0
phase_name "Zincite"
MVW( 0, 0, 0)
corrected_weight_percent 0
space_group P_63_M_C
scale @ 0.0001
K_Factor_WP( 0)
Phase_LAC_1_on_cm( 0)
Phase_Density_g_on_cm3( 0)
Hexagonal(@ 3.24974,@ 5.2066)
site Zn num_posns 0 x =1/3; : 0.3333333333 y =2/3; : 0.6666666667 z 0.00357 occ Zn+2 1 beq 0.5728
site O num_posns 0 x =1/3; : 0.3333333333 y =2/3; : 0.6666666667 z 0.37903 occ O-2 1 beq 0.5257
Preferred_Orientation(@, 1_LIMIT_MAX_1 min =0; max =1;,, 0 1 0)
xo_Is
LVol_FWHM_CS_G_L( 1, 0, 0.89, 0,,,@, 200)
xo @ 22.16326531
peak_type pv
pv_lor @ 0.5_LIMIT_MAX_1
pv_fwhm @ 1
I @ 24
wt_percent_K_MAC( 0) 'This macro reports phase amounts using the K-factor method'
for xdds { 'Instrument description for both XDDs'
lam ymin_on_ymax 0.0001
Lam_recs
{ 0.0159 1.534753 3.6854
0.5691 1.540596 0.4370
0.0762 1.541058 0.6000
0.2517 1.544410 0.5200
0.0871 1.544721 0.6200 }
LP_Factor(26.6)
Rp 173
Rs 173
Slit_Width(0.3)
Divergence (1)
axial_conv
filament_length 12
sample_length 15
receiving_slit_length 12
primary_soller_angle 4.6
secondary_soller_angle 4.6 }