Complex analysis of waste and industrial materials in the Laboratory ...

Complex analysis of waste
and industrial materials in the
Laboratory of X-Ray
Diffraction of ING PAN
dr Łukasz Kruszewski
Bruker axs D8 ADVANCE
VÅNTEC-1 LPS detector
• Linear Position Sensitive (superfast) detector
• VÅNTEC vs scintillation det.: ca. 100x better resolution
• very good peak-to-background intensity ratio
• 1s/step „standard” counting time 418s/step for VÅNTEC

Bruker axs D8 ADVANCE
• standard qualitative analysis of complex mixtures (ca. 3 min.
analysis)
• quantitative analysis of simple and complex mixtures incl. fly ash,
magnetic separates, clinkers, bricks, pyrometallurgic slags etc. (mainly
Rietveld method in TOPAS)
• determination of crystallinity degree and amorphous (glass) phase
content; unit cell parameters
• transmission geometry analysis of polytypes
• grazing incidence surface facture characteristics
• thermal chamber real-time phase transition analysis
Holders etc.
Calibration standards
LaB6

Additional equipment
Additional equipment
TOPAS – a complex tool for PXRD data analysis
• TOtal Powder Pattern decomposition (math. deconvolution)
• peak shape and whole profile fitting („repairing”)
• background corrections (Chebychev polynomials, 1/x function)
• sample preparation and sample-derived errors (sample
displacement, absorption, preferred orientation)
• instrument-derived errors (zero error, tangential correction,
untypical geometry)
LaB6 and Si – based calibration:

TOPAS – precise phase input data
• hkl phase Pawley or LeBail method (unit cell parameters, general fitting)
• structure phase full structure data (Rietveld quantitative analysis,
precise unit cell parameters calculation)
• peaks phase amorphous phase content determination
TOPAS – quantitative analysis –
iron-oxide-rich paralava of burning post coal-mining dump
low error
calculated unit cell
and other parameters
Very good fitting result
Good background statistics
full quantitative result
for 11 crystalline species
TOPAS – quantitative analysis –
crystallinity degree amorphous phase content
Precise calculation statistics information
Goodness of Fit (χ 2 )
Residual – weighted pattern
Durbin-Watson statistics

TOPAS – quantitative analysis – full text report
Quantitative Analysis - Rietveld
Phase 1 : "Fayalite magnesian" 30(410) %
Phase 2 : Diopside 7(86) %
Phase 3 : Hercynite 20(210) %
Phase 4 : Hematite 4(51) %
Phase 5 : "Bytownite An85" 6(250) %
Phase 6 : Magnesioferrite 1(1200) %
Phase 7 : Quartz 4(56) %
Phase 8 : "Mullite 3:2" 3(33) %
Phase 9 : "Tridymite low" 2(22) %
Phase 10 : Maghemite 20(230) %
Phase 11 : Indialite_KCa 6(85) %
Background
One on X 1(140000)
Chebychev polynomial, Coefficient 0 2400(3600)
1 -200(1800)
2 50(440)
3 20(100)
4 -13(23)
Corrections
Specimen displacement -0.117(11)
LP Factor 0
Absorption (1/cm) 24.5(40)
Structure 1
Phase name
Fayalite magnesian
R-Bragg 0.661
Spacegroup 62
Scale 0.000568(16)
Cell Mass 741.5(57)
Cell Volume (Å^3) 305.587(76)
Wt% - Rietveld 30(410)
Crystallite Size
Cry Size Lorentzian (nm) 176(20)
Crystal Linear Absorption Coeff. (1/cm) 216.1(17)
Crystal Density (g/cm^3) 4.029(31)
Preferred Orientation (Dir 1 : 3 0 -1) 0.918(14)
Lattice parameters
a (Å) 10.4423(15)
b (Å) 6.07677(92)
c (Å) 4.81578(65)
Site Np x y z Atom Occ Beq
s1 4 0.00000 0.00000 0.00000 FE+2 0.605(37) 0.41
MG+2 0.395(37) 0.41
s2 4 0.28000 0.25000 0.98610 FE+2 0.812(26) 0.36
MG+2 0.188(26) 0.36
s3 4 0.09720 0.25000 0.43070 SI+4 1 0.27
s4 4 0.09200 0.25000 0.76680 O-2 1 0.43
s5 4 0.45310 0.25000 0.21030 O-2 1 0.48
s6 8 0.16530 0.03630 0.28810 O-2 1 0.52
TOPAS – quantitative analysis –
white clinker (porcellanite) from post coal-mining burning dump
TOPAS – quantitative analysis –
synthetic mixture: Muscovite70Kaolinite10Quartz20
special peak type function used
for kaolinite and muscovite: PV_MOD

mri Thermal Chamber add
mri Thermal Chamber add – RESEARCH
(Bruker axs example)
mri Thermal Chamber add – RESEARCH
Bouna, L. and Rhouta, B. and Amjoud, M. and Maury, Francis and Lafont, Marie-Christine and Jada, A. and
Senocq, François and Daoudi, L. Synthesis, characterization and photocatalytic activity of TiO2 supported
natural palygorskite microfibers. (2011) Applied Clay Science, vol. 52 (n°3). pp. 301-311. ISSN 0169-1317

mri Thermal Chamber add – RESEARCH
Bouna, L. and Rhouta, B. and Amjoud, M. and Maury, Francis and Lafont, Marie-Christine and Jada, A. and
Senocq, François and Daoudi, L. Synthesis, characterization and photocatalytic activity of TiO2 supported
natural palygorskite microfibers. (2011) Applied Clay Science, vol. 52 (n°3). pp. 301-311. ISSN 0169-1317
mri Thermal Chamber add – RESEARCH
Bouna, L. and Rhouta, B. and Amjoud, M. and Maury, Francis and Lafont, Marie-Christine and Jada, A. and
Senocq, François and Daoudi, L. Synthesis, characterization and photocatalytic activity of TiO2 supported
natural palygorskite microfibers. (2011) Applied Clay Science, vol. 52 (n°3). pp. 301-311. ISSN 0169-1317
mri Thermal Chamber add – RESEARCH
FATIGUE BEHAVIOR OF PIEZOELECTRIC CERAMICS MATERIAL - Riffat Asim Pasha
03-UET/PhD-ME-03

mri Thermal Chamber add – RESEARCH
RONALD C. PETERSON AND ALAN H. GRANT 2005: DEHYDRATION AND CRYSTALLIZATION REACTIONS OF
SECONDARY SULFATE MINERALS FOUND IN MINE WASTE: IN SITU POWDER-DIFFRACTION EXPERIMENTS.
The Canadian Mineralogist, Vol. 43, pp. 1171-1181
mri Thermal Chamber add – RESEARCH
RONALD C. PETERSON AND ALAN H. GRANT 2005: DEHYDRATION AND CRYSTALLIZATION REACTIONS OF
SECONDARY SULFATE MINERALS FOUND IN MINE WASTE: IN SITU POWDER-DIFFRACTION EXPERIMENTS.
The Canadian Mineralogist, Vol. 43, pp. 1171-1181