Dear colleague! I send you the results of my tentative phase analysis. My participation number is SMRR-P021. Database: PDF file up to set 47 and about 26000 phases calculated using data about crystal structure of intermetallic compounds (P.Villars, L.D.Calvert. Pearson's Handbook of Crystallographic Data for Intermetallic Phases. - American Society for Metals, v.1-3, 1985, 3260 p) and selected phases from Inorganic Crystal Structure Database (Karlsruhe). Program(s): package of DOS-programs developed by E.V.Shelekhov (Moscow Institute of Steel and Alloys, X-ray Department). Phases are selected by program PHAN (program of qualitative phase analysis) using next criteria: - nature of phase (Inorganic, organic, mineral, alloy); - chemical composition (if known); - P - intensity threshold for peaks to be taken into account; - tolerance window over d: delta(d)=c*d^n The main criterion is so called "overlapping" - scalar product of experimental and phase patterns (in functional analysis sense, i.e. integral over the diffraction vector of one pattern multiplied by another), normalized by lengthes of both patterns. In other words, it is cos(phi), where phi is the "angle" between two patterns. To accelerate calculations both pattern are represented as sets of peaks with squared Cauchy profile (position, height, FWHM), basing on which the overlapping is produced analytically. The overlapping is used while searching the main phases. Basing on main phases an iterative procedure can be applied to search additional phases, which uses the scalar products of patterns as well, and then, in turn, additional phases can be transferred into main ones and the procedure repeated. SAMPLE 1. phase composition: FeCO3 Ca5 (P O4)3 (OH) (or other compound like apatite) Si O2 (alpha-quarzt) Fe3 Al4 (PO4)4 (OH)6 * 2 H2 O (36-403) All these phases were identified using following values of search parameters: Chemical composition: Fe,P,O,Ca and dopants Si,H and Al Search of main phases with parameters: P=20% c=0.003, n=2 overlapping (normalization for the local one is done over the tolerance windows around sticks of phase stick-diagram): S(local)=0.4 S(total)=0.2 Two phases have been identified - FeCO3 and Si O2. The rest of phases has been found in "additional phases" searching mode. Volume fractions of these phases are estimated using quantitative phase analysis program PHAN% (full profile refinement by simplified Rietveld method). Volume fractions of the phases are shown below: Phase Vol.frac., % Fe C O3 ( type G01 ) 36 Ca5 (P O4)3 F (apatite) 42.9 Si O2 ( type C8 ) 18.6 Fe3 Al4 (PO4)4 (OH)6 * 2 H2 O 2.5 The phase Fe3 Al4 (PO4)4 (OH)6 * 2 H2 O is from PDF and has no corundum number, so the absolute intensity of its strongest peak is incommensurate with those of other phases the patterns of which have been calculated. Therefore the volume fraction of last phase may be multiplied by some factor. Sample 2. There is no similar phase in our database (up to 47-th set of PDF) The pattern was indexed and proved to be the single-phase one with tetragonal crystal structure and lattice parameters a=9.092 ang. and c=13.47 ang. (d/n)exp. ( H K L ) (d/n)calc 1 7.531 ( 1 0 1 ) 7.536 2 4.647 ( 1 1 2 ) 4.650 3 4.552 ( 2 0 0 ) 4.546 4 4.022 ( 1 0 3 ) 4.026 5 3.892 ( 2 1 1 ) 3.893 6 3.770 ( 2 0 2 ) 3.768 7 3.370 ( 0 0 4 ) 3.367 8 3.215 ( 2 2 0 ) 3.215 9 3.013 ( 2 1 3 ) 3.014 10 2.983 ( 1 1 4 ) 2.983 11 2.959 ( 3 0 1 ) 2.957 12 2.898 ( 2 2 2 ) 2.901 13 2.876 ( 3 1 0 ) 2.875 14 2.706 ( 2 0 4 ) 2.706 15 2.644 ( 3 1 2 ) 2.644 16 2.582 ( 1 0 5 ) 2.583 17 2.511 ( 3 0 3 ) 2.512 18 2.478 ( 3 2 1 ) 2.479 19 2.327 ( 2 2 4 ) 2.325 20 2.273 ( 4 0 0 ) 2.273 21 2.246 ( 2 1 5 ) 2.246 22 2.199 ( 3 2 3 ) 2.199 23 2.188 ( 3 1 4 ) 2.187 24 2.176 ( 4 1 1 ) 2.176 25 2.151 ( 4 0 2 ) 2.154 26 2.032 ( 4 2 0 ) 2.033 27 2.014 ( 3 0 5 ) 2.013 28 1.979 ( 4 1 3 ) 1.979 29 1.882 ( 1 0 7 ) 1.883 30 1.841 ( 3 2 5 ) 1.841 31 1.802 ( 5 0 1 ) 1.802 ( 4 3 1 ) 32 1.783 ( 5 1 0 ) 1.783 33 1.770 ( 3 1 6 ) 1.769 34 1.740 ( 4 2 4 ) 1.740 35 1.705 ( 4 1 5 ) 1.706 36 1.684 ( 0 0 8 ) 1.684 37 1.675 ( 5 2 1 ) 1.675 Sample 3 The phase composition is admittedly: C13 H10 N2 O JCPDS 19-1946 (N O2)2 C6 H4 JCPDS 31-1675 C6 H4 O6 * 2 H2 O JCPDS 41-1938 C9 H9 N O JCPDS 20-1762 C13 H9 N O JCPDS 45-1544 and one (or more) unidentified phase.... The phases C13 H10 N2 O, (N O2)2 C6 H4 and C9 H9 N O was found with parameters: P=30% c=0.003, n=10 S(local)=0.4 S(total)=0.2 The rest of phases has been found as "additional phases". Phase Pseudo-volume fraction, % C13 H10 N2 O 49.4 (N O2)2 C6 H4 7.5 C6 H4 O6 × 2 H2 O 7.8 C16 H14 N2 O8 22.0 C9 H9 N O 5.3 C13 H9 N O 8.1 sample 4. Phase composition of this sample was identified on the first step of Search-Match Round Robin-2002. phase composition: Pb O Pb S O4 * 4Pb O (Pb O)3 Pb S O4 * H2 O Phases Pb O and Pb S O4 * 4Pb O were identified using following values of search parameters: Nature - Inorganic, exclude Organic phases and Replaced cards P=35% c=0.003, n=2 S(local)=0.7 S(total)=0.5 To identify the phase (Pb O)3 Pb S O4 * H2 O the chemical composition is set as Pb in combination with arbitrary another elements. Search parameters are: P=90% c=0.0035, n=2 S(local)=0.5 S(total)=0.3 Volume fractions of the phases are shown below: Phase Vol.fract., % Pb O ( type B10 ) 42 Pb S O4 * 4 Pb O 44 (Pb O)3 Pb S O4 * H2 O 14 To improve the goodness of fitting the texture parameters are used for the phase Pb S O4 * 4 Pb O.