SMRR-2002 results

Best seen in 1024x768 resolution or higher
Last update - July 2002
Jean-Marc Le Meins - Lachlan M. D. Cranswick - Armel Le Bail


Content :
Official solutions
From the participants to Step 1 (knowledge limited to sample origin)
From the participants to Step 2 (with chemical content)
Conclusions
    Step 1
    Step 2
General conclusion
Post-deadline comments from participants


Official solutions
 
Sample 1 Sample 2 Sample 3 Sample 4
Sample history
Screen copy
15-0876 Fluorapatite
12-0531 Siderite
36-0403 Gormanite
33-1161 Quartz
+ uncertain trace(s)
Souzalite forming a series with gormanite is acceptable, as well as MgCO3 or (Fe,Mg)CO3 in place of Fe(CO3), and hydroxylapatite
Sample history
Screen copy
48-0475 Octadecasil...
- in fact : similar to - with small difference on cell parameters and close intensities
Sample history
Screen copy
19-1946 Thalidomide 
This is alpha thalidomide
+ phase not in the PDF which is beta-thalidomide (mixture 50% of each polymorph).
Sample hstory
Screen copy
05-0561 Litharge PbO
23-0333 Pb5O4SO4...
29-0781 Pb4O3SO4.H2O
38-1477 Massicot PbO
+ traces of :
33-1486 Lanarkite
05-0577 Anglesite
13-0131 Hydrocerussite
04-0686 Lead

Comments :
- Real-life samples have certainly not always exact solutions in the PDF. A search-match program should be efficient enough to give the maximum fits.
- It was said at the SMRR Web page that "the PDF contains solutions or at least close solutions to these problems". We recognize that "close" was meaning close to 50% in our mind for the thalidomide case. So that, yes, there were some pitfalls in the SMRR, mainly for samples 2 and 3 (moreover, the thalidomide molecular formula is false into the 19-1946 PDF card - C13H10N2O instead of C13H10N2O4).
- More than 200 downloads of the data occured, for finally 25 participants to step 1 below.

Data may still be downloaded for your own post-SMRR tests.



From the participants to step 1 (knowledge limited to sample origin)

JCPDS-ICDD card number in bold means correct identification (multiple cards are available for quartz, apatite, lead oxide, etc). Note that proposals not in bold are not necessarily always false : they may correspond to minor phases difficult to ascertain.
... means the name or formula is truncated for lack of room in this page
 
Participant/Program/ICDD Sample 1 Sample 2 Sample 3 Sample 4
P1 
EVA - Socabim/Bruker
ICDD release 2001
More stuff (.txt)
Even more stuff (.pdf)
Screen copy
84-1997 Fluorapatite
83-1764 Siderite
46-1045 Quartz
36-0403 Gormanite
42-0581 Alluaudite
Screen copy
48-0475 Octadecasil...
Screen copy
19-1946 Thalidomide
45-1544 6-Amino-phen...
48-2830 N-Butyl-p-nit...
47-2262 Tri(benzimid...
30-1806 Methyl diphe...
Screen copy
05-0561 Litharge
23-0333 PB5O4SO4...
29-0781 Pb4O3SO4.H2O
P2
EVA 7 - Socabim/Bruker
ICDD release 2001
More stuff (.txt)
Screen copy
85-0335 Quartz
15-0876 Fluorapatite
Screen copy
19-1946 Thalidomide
Screen copy
78-1666 Lead Oxide - PbO
23-0333 Pb5O4SO4...
88-0552 (PbO)3PbSO4.H2O
P3
JADE V6.1 - MDI
ICDD release 2001 - set 51
More stuff (.txt)
Screen copy
29-0696 Siderite
36-0403 Gormanite
46-1045 Quartz
15-0876 Fluorapatite
08-0098 Lepidocricite
Screen copy
48-0475 Octadecasil
Screen copy
05-0561 Litharge
23-0333 Pb5O4SO4...
29-0781 Pb4O3SO4.H2O
P4
HighScore v.1.0b - Philips
ICDD release 2001
More stuff (.txt)
Screen copy
86-0740 Hydroxylapatite
78-1254 Quartz
81-0591 Zircon
42-1397 Girvasite
80-1306 Amarilliite
36-0403 Gormanite
Screen copy
26-1993 C8H20NF6U
Screen copy
05-0561 Litharge
05-0570 Massicot
23-0333 Pb5O4SO4...
29-0781 Pb4O3SO4.H2O
P5
EVA 6 - Socabim/Bruker
ICDD release 2000
More stuff (.txt)
Screen copy
46-1045 Quartz
29-0696 Siderite
15-0876 Fluorapatite
36-0403 Gormanite
Screen copy Screen copy
19-1946 Thalidomide
48-2011 Poly(4-pentame...
18-0335 Cesium Borate...
Screen copy
05-0561 Litharge
23-0333 Pb5O4SO4...
88-0552 (PbO)3PbSO4.H2O
P6
EVA - Socabim/Bruker
ICDD release not given
More stuff (.txt)
Screen copy
15-0876 Fluorapatite
12-0531 Siderite
36-0403 Gormanite
33-1161 Quartz
xx-0377 Ferroalluaudite
Screen copy
19-1946 Thalidomide
45-1544 6-Amino-phenale...
Screen copy
23-0333 Pb5O4SO4...
05-0561 Litharge
29-0781 Pb4O3SO4.H2O
P7
Philips Graphics & Identify
ICDD release 2000
More stuff (.txt)
Screen copies provided after the deadline
Screen copy
73-1727  Fluorapatite
86-2237  Quartz, low
12-0088  Ankerite
83-1764  Siderite
Screen copy Screen copy
18-1940  Tetrakis thiourea...
41-1610  Glucose sodium...
19-1946  Thalidomide
28-1734  Nickel ethylene...
Screen copy
23-0333 Pb5O4SO4...
87-0604 Litharge
38-1477 Massicotite
P8
JADE 5 - MDI
ICDD release not given
More stuff (.txt)
Screen copy
88-2302 Quartz
36-0403 Gormanite
71-0880 Fluorapatite
83-1764 Siderite
Screen copy
48-0475 Octadecasil...
Screen copy
19-1946 Thalidomide
Screen copy
85-1739 Litharge
29-0781 Pb4O3SO4.H2O
23-0333 Pb5O4SO4...
P9
Diffract-At v3.0 - Socabim
ICDD release 2000
More stuff (.txt)
No screen copy
71-0880 Fluorapatite
85-0335 Quartz
86-2348 Mg(CO3)
No screen copy
88-1173 TiO2
No screen copy
19-1946 Thalidomide
07-0710 6-Amino-2thio...
No screen copy
05-0561 PbO
23-0333 Pb5O4SO4...
P10
FARHAN
ICDD mineral files set 1-45
More stuff (.txt)
Screen copy
29-0696 Siderite
19-0272 Ca/hydroxylapatite
33-1161 Quartz
45-1349 Haynesite
25-0676 Mountainite
P11
EVA - Socabim/Bruker
ICDD release not given
More stuff (.txt)
Screen copy
86-0740 Hydroxylapatite
78-1254 Quartz
82-1815 Sodalite
Screen copy
48-0475 Octadecasil
Screen copy
87-0604 Litharge, syn
23-0333 Pb5O4SO4...
88-0552 Pb4O3SO4.H2O
P12
Eva - Socabim/Bruker
ICDD release 2001
More stuff (.txt)
No screen copy
85-0335 Low Quartz
84-1997 Fluorapatite
83-1764 Siderite
33-0863 Souzalite
No screen copy
48-0475 Octadecasil
No screen copy
05-0561 Litharge
23-0333 Pb5P4SO4...
88-0552 Pb4O3SO4.H2O
73-1056 Parabutlente
P13
Eva (??) - Socabim/Bruker
ICDD release not given
More stuff (.txt)
Screen copy
46-1045 Quartz
29-0696 Siderite
33-0863 Souzalite
46-1212 Al2O3
15-0876 Fluorapatite
Screen copy
46-0099 Copper Aluminium...
02-0770 Cobalt oxide
42-1678 Betaine borate
78-0521 Lead Bismuth...
41-1487 Graphite-2H
39-1425 Cristobalite
04-0857 Griceite
36-0426 Dolomite
Screen copy
45-1544 6-Amino-phen...
33-2000 Quinupramine...
42-1677 Betaine Phosphate
44-1626 1,3,5-Trinitro...
79-0867 Hydreous Ruthe...
19-1946 Thalidomide
47-1925 N-(2,3-Dihydro...
Screen copy
05-0561 Litharge
23-0333 Pb5O4SO4...
38-1477 Massicot
73-1058 Parabutlerite
82-2454 Sengierite
P14
Bede Search/Match for 1 & 4
Hanawalt for sample 2
ICDD release 2001
More stuff (.txt)
No screen copy
03-0747 Hydroxylapatite
77-1060 Quartz
83-1764 Siderite
80-1296 Na2Ca6(Si2O7)...
No screen copy
48-0475 Octadecasil
No screen copy
35-1482 Litharge
23-0333 Pb5O4SO4...
29-0781 Pb4O3SO4.H2O
P15
EVA 6 - Socabim/Bruker
ICDD release 2000
More stuff (.txt)
Even more stuff (.pdf)
Screen copy
29-0696 Siderite
33-0863 Souzalite
46-1045 Quartz
82-1429 Hydroxylapatite
44-1415 Lepidocrocite
Screen copy
48-0475 Octadecasil
Screen copy
19-1946 Thalidomide
Screen copy
05-0561 Litharge
23-0333 Pb5O4SO4...
88-0552 Pb4O3SO4.H2O
38-1477 Massicot
P16
EVA - Socabim/Bruker
ICDD release not given
More stuff (.txt)
No screen copy
Fluorapatite
Siderite
Screen copy
Pattern indexed + Le Bail fit
Tetragonal, a = 9.0805 
                  c = 13.4539 
No screen copy
19 1946 Thalidomide
+ probable:  31-1701,   36-1887,   42-1667,   48-2285,   50-2015, 
42-1564,   45-1997.
Screen copy
05-0561 Litharge
23-0333 Pb5O4SO4...
29-0781 Pb4O3SO4.H2O
P17
EVA 5 - Socabim/Bruker
ICDD up to set 47
More stuff (.txt)
Screen copy
46-1045 Quartz
15-0876 Fluorapatite
46-1388 Arupite
33-0863 Souzalite
37-0447 Clinoclase
Screen copy
02-0770 Cobalt Oxide
Screen copy
19-1946 Thalidomide
Screen copy
05-0561 Litharge
23-0333 Pb5O4SO4...
P18
JADE 5.1 - MDI
ICDD release not given
Screen copy
05-0561 Litharge
23-0333 Pb5O4SO4...
38-1477 Massicot
29-0781 Pb4O3SO4.H2O
P19
Retrieve based on query language for XRD phase identification (Igor Yakimov). ICDD up to set 47
Screen copy
46-1045 Quartz
29-0696 Siderite
15-0876 Fluorapatite
36à0403 Gormanite
42-0581 Alluaudite
33-0664 Hematite
Screen copy Screen copy
19-1946 Thalidomide
Screen copy
05-0561 Litharge
23-0333 Pb5O4SO4...
29-0781 Pb4O3SO4.H2O
38-1477 Massicot
08-0087 Fe3O4
P20
CSM - Oxford Cryosystems
ICDD up to set 51 
More stuff (.txt)
No screen copy
15-0876 Apatite
83-2245 Quartz
36-0403 Gormanite
79-1346 Dolomite
71-2225 Zn(N3)2(NH3)2
No screen copy
48-0475 Octadecasil
26-1993 C8H20NF6U
No screen copy
72-1663 NaHCO3
09-0432 Hydroxylapatite
No screen copy
35-1482 PbO
23-0333 Pb5O4SO4...
88-0551 Pb4O3SO4.H2O
P21
PHAN by E.V.Shelekhov ICDD up to set 47
More stuff (.txt)
Screen copy
15-0876 Fluorapatite
29-0696 Siderite
46-1045 Quartz
Screen copy
xx-xxxx  Zn[C(NH2)3]2...
Cell parameters determined a=9.092 ang. ; c=13.47 ang.
Screen copy
19-1946 Thalidomide
31-1670 C7H12O4
23-1523 CH3N5.H2O
32-1527 C8H7NO
Screen copy
23-0333 Pb5O4SO4...
xx-xxxx PbO
xx-xxxx Pb4O3SO4.H2O
P22
EVA 7 - Socabim/Bruker
ICDD release 1999
More stuff (.txt)
Screen copy
76-0558 Fluoroapatite 
76-0228 Berlinite
29-0696 Sidenite 
44-1415 Lepidocrocite 
33-0863 Souzalite 
Screen copy
81-1573 Lithium Alumin...
76-1608 TlGaF6
83-1769 Rb2Hg(CN)4
34-1440 CaNbF7
Screen copy
23-0333 Pb5O4SO4...
29-0781 Pb4O3SO4.H2O
78-1666 PbO
P23
JADE 5 - MDI
ICDD release 2000
More stuff (.txt)
Screen copy
46-1045 Quartz, syn
73-1727 Fluoroapatite
83-1764 Siderite
36-0403 Gormanite
Screen copy
48-0475 Octadecasil
Refined cell  a = 9.08367(2), b = 13.4606(7)
Screen copy
19-1946 Thalidomide
39-1917 Antabuse
39-1841 Sulfadiazine
Screen copy
85-1739 Litharge
29-0781 Pb4O3SO4.H2O
23-0333 Pb5O4SO4...
P24
Philips Graphics & Identify ICDD release 2000
More stuff (.txt)
Screen copy
30-0276 Ca4Sm6O2(PO4)...
77-0120 Ca5F(PO4)3
72-1140 Li2SiO3
50-1301 Sm2Se3
Screen copy
26-1993 C8H20NF6U
Screen copy
85-2433 Na2.667Nb6P4O...
Screen copy
80-1934 Ca2Ho(RuO6) 
50-1779 Nd2Y2O3F6 
84-1029 TaNi3S8 
84-1022 Cs3Cr2Br9 
23-0333 Pb5O4SO4
35-1482 PbO
P25
Philips Graphics & Identify
ICDD release 1999 (set 49)
More stuff (.txt)
Screen copy
15-0876 Fluorapatite
46-1045 Quartz
29-0696 Siderite
33-0863 Souzalite
Screen copy
19-1946 Thalidomide
37-1587 C5H10N2O3
Screen copy
23-0333 Pb5O4SO4...
35-1482 PbO

Comments :
- Many participants could not identify sample 2 because they were using an old ICDD release not including the 48-0475 card.
- The CSM (Crystallographica Search Match from Oxford Cryosystems) core is now included into the Philips Highscore program



From the participants to step 2 (with chemical content)

Comments :
To those complaining about the C13H10N2O4 given formula not matching the Thalidomide 19-1946 with C13H10N2O formula, it was replied that "PDF is not free of error".
 
Participant/Program/ICDD Sample 1 Sample 2 Sample 3 Sample 4
P3 - No change
JADE V6.1 - MDI
ICDD release 2001 - set 51
More stuff (.txt)
Screen copy
29-0696 Siderite
36-0403 Gormanite
46-1045 Quartz
15-0876 Fluorapatite
08-0098 Lepidocricite
Screen copy
48-0475 Octadecasil
Screen copy
05-0561 Litharge
23-0333 Pb5O4SO4...
29-0781 Pb4O3SO4.H2O
P4
HighScore v.1.0b - Philips
ICDD release 2001
More stuff (.txt)
Screen copy
36-0403 Gormanite
78-1254 Quartz
75-0783 Corundum
87-2462 Fluorapatite
Screen copy
48-0475 Octadecasil
Screen copy
19-1946 Thalidomide
Screen copy
05-0561 Litharge
05-0570 Massicot
23-0333 Pb5O4SO4...
29-0781 Pb4O3SO4.H2O
19-0682 Pb2OCO3
05-0417 Cerussite
P5
EVA 6 - Socabim/Bruker
ICDD release 2000
More stuff (.txt)
Screen copy
46-1045 Quartz
29-0696 Siderite
15-0876 Fluorapatite
36-0403 Gormanite
Screen copy
29-0085 SiO2 
Screen copy
19-1946 Thalidomide
Screen copy
05-0561 Litharge
23-0333 Pb5O4SO4...
88-0552 (PbO)3PbSO4.H2O
P7
Philips Graphics & Identify
ICDD release 2000
More stuff (.txt)
Screen copy
82-1429  Hydroxylapatite
86-2237  Quartz, low
76-0227 Berlinite
83-1764  Siderite
Screen copy
23-0333 Pb5O4SO4...
87-0604 Litharge
72-0151 Massicotite
P8
JADE 5 - MDI
ICDD release not given
More stuff (.txt)
Screen copy
85-1054 Quartz
83-1764 Siderite
86-0740 Hydroxylapatite
36-0403 Gormanite
Screen copy (no change)
48-0475 Octadecasil...

 

Screen copy (no change)
19-1946 Thalidomide

 

Screen copy (no change)
85-1739 Litharge
29-0781 Pb4O3SO4.H2O
23-0333 Pb5O4SO4...
P9
Diffract-At v3.0 - Socabim
ICDD release 2000
More stuff (.txt)
Screen copy
83-1764 Siderite
78-1254 Quartz
86-0740 Hydroxylapatite
36-0403 Gormanite
Screen copy
70-0273 (NH4)2SiP4O13
Screen copy
19-1946 Thalidomide
07-0710 6-Amino-2thio...
31-1809 N-1-Naphthyl...
Screen copy
05-0561 PbO
23-0333 Pb5O4SO4...
88-0552 (PbO)3PbSO4.H2O
P10
FARHAN
ICDD mineral files set 1-45
More stuff (.txt)
Screen copy
29-0696 Siderite
19-0272 Ca/hydroxylapatite
33-1161 Quartz
39-1425 Cristobalite
41-1355 Scolecite
41-1475 Aragonite
P11
EVA - Socabim/Bruker
ICDD release not given
More stuff (.txt)
Screen copy
86-0740 Hydroxylapatite
85-0794 SiO2
83-1764 Siderite
76-1846 Wollastonite
24-0222 Ca(Zn(OH)3)2....
74-0836 Xanthophyllite
Screen copy
48-0475 Octadecasil
Screen copy
Alpha-thalidomide
Beta-Thalidomide

from CSD

Screen copy
87-0604 Litharge, syn
23-0333 Pb5O4SO4...
88-0552 Pb4O3SO4.H2O
P12
Eva - Socabim/Bruker
ICDD release 2001
More stuff (.txt)
No screen copy
85-0335 Low Quartz
84-1997 Fluorapatite
83-1764 Siderite
No screen copy
48-0475 Octadecasil
Screen copy
19-1946 Thalidomide
72-0118 Urea
38-1715 Thamocifen citrate
36-1546 Vanillin
No screen copy
05-0561 Litharge
23-0333 Pb5P4SO4...
88-0552 Pb4O3SO4.H2O
P13
Eva (??) - Socabim/Bruker
ICDD release - set 1-48
More stuff (.txt)
Screen copy
46-1045 Quartz
29-0696 Siderite
46-1212 Al2O3
09-0432 Hydroxylapatite
36-0403 Gormanite
Screen copy
19-1946 Thalidomide
45-1544 6-Amino-phen...
44-1626 1,3,5-Trinitro...
17-0967 Anhydrotetro...
22-1862 N-(p-Nitrophenyl...
28-1622 3,7-Diacetyl-1,3...
Screen copy
05-0561 Litharge
23-0333 Pb5O4SO4...
38-1477 Massicot
29-0781 Pb4O3SO4.H2O
P14
Bede Search/Match for 1 & 4
Hanawalt for sample 2
ICDD release 2001
More stuff (.txt)
No screen copy
03-0747 Hydroxylapatite
77-1060 Quartz
83-1764 Siderite
26-1381 Ca3Al6.5Si11.5...
No screen copy
48-0475 Octadecasil

(Hanawalt search)

No screen copy

See text

No screen copy
35-1482 Litharge
23-0333 Pb5O4SO4...
29-0781 Pb4O3SO4.H2O
P16
EVA - Socabim/Bruker
ICDD up to set 50
More stuff (.txt)
No screen copy
Siderite
Fluorapatite
Moganite
Quartz
Screen copy
48-0475 Octadecasil
Screen copy
19-1946 Thalidomide
Screen copy
05-0561 Litharge
23-0333 Pb5O4SO4...
29-0781 Pb4O3SO4.H2O
P17
EVA 5 - Socabim/Bruker
ICDD up to set 47
More stuff (.txt)
Screen copy
29-0696 Siderite
46-1045 Quartz
36-0403 Gormanite
Screen copy
05-0561 Litharge
23-0333 Pb5O4SO4...
29-0781 Pb4O3SO4.H2O
P19
Retrieve based on query language for XRD phase identification (Igor Yakimov). ICDD up to set 49 
More stuff (.txt)
Screen copy (no change)
46-1045 Quartz
29-0696 Siderite
15-0876 Fluorapatite
36à0403 Gormanite
42-0581 Alluaudite
33-0664 Hematite
Screen copy
48-0475 Octadecasil
Screen copy (no change)
19-1946 Thalidomide
Screen copy (no change)
05-0561 Litharge
23-0333 Pb5O4SO4...
29-0781 Pb4O3SO4.H2O
38-1477 Massicot
08-0087 Fe3O4
P20
CSM - Oxford Cryosystems
ICDD up to set 51 
More stuff (.txt)
Screen copy
15-0876 Apatite
46-1045 Quartz
36-0403 Gormanite
79-1346 Dolomite
Screen copy
48-0475 Octadecasil
26-1993 C8H20NF6U
Screen copy
19-1946 Thalidomide
51-2367 C15H13N3O4 
Screen copy
05-0561 Litharge
23-0333 Pb5O4SO4...
88-0552 Pb4O3SO4.H2O
P21
PHAN by E.V.Shelekhov ICDD up to set 47
More stuff (.txt)
Screen copy
46-1045 Quartz
29-0696 Siderite
09-0432 Hydroxylapatite
36-0403 Gormanite
Cell parameters determined a=9.092 ang. ; c=13.47 ang. Screen copy
19-1946 Thalidomide
31-1675 (NO2)2C6H4
28-1762 C9H9NO
41-1938 C6H4O6.2H2O
45-1848 C16H14N2O8
Screen copy
23-0333 Pb5O4SO4...
xx-xxxx PbO
xx-xxxx Pb4O3SO4.H2O
P22
EVA 7 - Socabim/Bruker
ICDD release 1999
More stuff (.txt)
Screen copy
76-0558 Fluoroapatite 
76-0228 Berlinite
29-0696 Siderite 
44-1415 Lepidocrocite 
33-0863 Souzalite 
82-0511 Quartz
Screen copy
48-0475 Octadecasil
Screen copy
23-0333 Pb5O4SO4...
29-0781 Pb4O3SO4.H2O
78-1666 PbO
P23
JADE 5 - MDI
ICDD release 2000
More stuff (.txt)
Screen copy
46-1045 Quartz, syn
36-0403 Gormanite
09-0432 Hydroxylapatite
83-1764 Siderite
Screen copy
48-0475 Octadecasil
Refined cell  a = 9.08367(2), b = 13.4606(7)
Screen copy
19-1946 Thalidomide
Screen copy
85-1739 Litharge
29-0781 Pb4O3SO4.H2O
23-0333 Pb5O4SO4...
22-1134 3PbO.H2O
P24
Philips Graphics & Identify ICDD release 2000
More stuff (.txt)
No screen copy
86-0740 Ca(PO4)3(OH)
76-0271 H3PO3
83-0460 Ca2(SiO4)
74-1733 Ca2FeAl2Si3O12... 
72-1441 AlSiO5
81-1592 Si5(PO4)6O
88-0436 Ag2(VP2O8).
No screen copy
48-0475 Octadecasil
45-1374 SiO2
SiF4
No screen copy
19-1946 Thalidomide
No screen copy
23-0333 Pb5O4SO4
35-1482 PbO
88-0552 Pb4O3SO4.H2O
New participants
P26
EVA - Socabim/Bruker
ICDD release 2000
More stuff (.txt)
Screen copy
46-1045 Quartz
29-0696 Siderite
36-0403 Gormanite
09-0432 Hydroxylapatite
Screen copy
48-0475 Octadecasil
Sreen copy
19-1946 Thalidomide
Screen copy
23-0333 Pb5O4SO4
05-0561 Litharge
29-0781 Pb4O3SO4.H2O
38-1477 Massicot (.txt)
P27
Traces v5
ICDD release 1999
More stuff (.txt)
No screen copy
Quartz
Siderite
Hydroxylapatite
gormanite
No screen copy
stishovite
quartz
SiF4
SiO2
No screen copy
Thalidomide
No screen copy
Litharge
Pb4O3SO4.xH2O
Pb5O4SO4
P28
EVA - Socabim/Bruker
ICDD release up to set 46
Screen copy
29-0696 siderite
46-1045 Quartz
09-0432 Hydroxylapatite
36-0403 Gormanite
Screen copy
05-0561 Litharge
23-0333 Pb5O4SO4...
35-1482 PbO
29-0781 Pb4O3SO4.H2O
P29
Graphics & Identify - Philips
ICDD release not given
More stuff (.txt)
Screen copy
86-2237 Quartz
83-1764 siderite
36-0403 Gormanite
75-0915 Fluorapatite
Screen copy
48-0475 Octadecasil
Screen copy
87-0604 Litharge
29-0781 Pb4O3SO4.H2O
P30
HighScore - Philips
ICDD release not given
More stuff (.txt)
Screen copy
79-1910 Quartz
83-1764 Siderite
86-0740 Hydroxylapatite
33-0638 Gormanite
74-1877 Lepidicrocite
03-0251 Goethite
25-0119 Crandallite
85-1569 Garronite
Screen copy
87-0604 Litharge
74-1038 Enargite
71-2438 Talnakhite
23-0333 Pb5O4SO4...
04-0461 Matlockite
80-1390 Leadhillite
84-2035 Pahasapaite



Conclusions

Step-1

Three main software packages were used by the participants in step 1 of the SMRR (see figure below): Jade, from MDI, (16%); X'Pert Graphic & Identify, from Philips (12%); and EVA from Socabim / Bruker (48%). There was only one participant using each of the 6 other packages.

The table below shows the versions of the ICDD-PDF used by the participants. 56% of them used a release from 1999 at least. This number is probably higher because 28% of the participants did not give this information. So that at least 16% of the participants could not identify sample 2 (card 48-0475) because they were using a too old ICDD release.

Some answers do not include all samples but 92% of the participants give at least their answers for 3 samples. A summary of the results is proposed in the following table:


I stands for indexed pattern only.

If we should have a winner at step 1, this would be Participant 15, the only one having proposed the 10 right phases for the four samples, using EVA (Socabim/Bruker). However, some participants could have declared for some samples (see their original texts above) : "prefer to wait for chemical information for this sample", or "nothing found that would be reasonable for this sample" or "no experience with organic compounds, I prefer not to participate for this sample" so that some participants could be considered as winners for the part of the challenge selected by themselves (because, it was not an obligation to return results for all samples). If Participant 19 have had a recent ICDD release allowing to cope with sample 2, he may have also win that SMRR, since he could identified the 9 other phases. And P18 who participated only for sample 4 found the 4 phases, is also a kind of winner.

We have not really enough participants using the same software in order to discuss the results according to the user experience, with the exception of EVA, maybe. Nine different software were used in this Search-Match Round Robin. The mean number of phases identified for each sample is given below (nr = no result provided ; id = incomplete database precluding sample 2 identification), and also the numbers given by the best performer (mixing the software versions) and the worst one.
 
Software Participants Sample 1 Sample 2 Sample 3 Sample 4
EVA - Socabim/Bruker P1, P2, P5, P6, P9, P11, P12
P13, P15, P16, P17, P22
3.33/4 - 4/4 - 2/4 0.50/1 - 1/1 - 0/1 0.75/1 - 1/1 - 0/1 2.92/4 - 4/4 - 2/4
JADE - MDI P3, P8
P18 (nr for samples 1,2,3), P23
4/4 - 4/4 - 4/4 1/1 - 1/1 - 1/1 0.75/1 - 1/1 - 0/1 3.25/4 - 4/4 - 3/4
Highscore - Philips P4 3/4 0/1 0/1 4/4
Graphics & Identify - Philips P7, P24, P25 2.67/4 - 4/4 - 1/4 0/1 - 0/1 - 0/1 0.67/1 - 1/1 - 0/1 2.33/4 - 3/4 - 2/4
FARHAN P10 3/4 nr nr nr
Bede Search/Match P14 3/4 1/1 (Hanawalt) 0/1 3/4
Yakimov P19 4/4 id 1/1 4/4
CSM - Oxford Cryosystems P20 4/4 1/1 0/1 3/4
PHAN P21 3/4 id 1/1 3/4

These results as a whole indicate that in the absence of details about the chemistry, but including informations allowing to select a subset (mineral, inorganic...), the performance of the above search-match software is quite high. All the above programs appear to be able to identify 3-4  phases in a mixture of up to 4 major phases. From the series of EVA users, the performance appears to depend a lot on the performer training, and this seems to be particularly true for the more difficult samples 2 (no exact match possible - only close match) and 3 (no complete match possible - only one of the two polymorphs is in the PDF). We certainly cannot conclude to a "best program" from these very limited results (moreover, a dozen of programs have not participated to the SMRR, and there is not enough participants using the same package). The reader will have to make his own conclusion.
Indeed, it is sometimes a clear advantage to be able to identify phases in a sample without doing any chemical analysis : if you can trust the identification and if you conclude that there is no necessity in doing any further chemical analysis (for the sample has no interest, or for any other reason), then you can save time and money. Moreover, performing a chemical analysis of a fine powder which is eventually a phase mixture will give you only a global composition, no detail on the individual phases, of course. OK, if you are the synthesis performer, you know already what elements are inside the sample. But sometimes, you are not the synthesis performer : the sample may be natural, or manufactured at ancient times, or maybe something unexpected occured during the synthesis (error in selecting the starting reagents, contamination by the containers, etc).



Step 2

The more confusing case in this SMRR is sample 3 for which the maximum of information was given at step 2 : a mixture of C13H10N2O4 polymorphs. In fact, there was no problem at all here, since the full solution was there already : a mixture of thalidomide polymorphs.  In spite of this, many participants declare "the compound is not present in the PDF" (because of the C13H10N2O wrong formula of the 19-1946 thalidomide card, matching only half the pattern, but proposed by most of the search-match software in first position)  or "There is only one pattern with the molecular formula C13H10N2O4 (02-0201) in PDF release 1999 and it is not present in this diffraction pattern." or they continue to propose phases having compositions different from the given one, etc. Some Participants are trusting so much the PDF that they can't imagine any error inside of it (more probably there are hundreds or possibly thousands of -small- errors inside it). More incredible, some obtained the good identification at step 1, but not at step 2. Only one full winner for sample 3 proposed the identification of the 2 thalidomide polymorphs from CSD data : P11.

Some excellent participants at Step 1 obviously decided not to participate to Step 2. This may be because they did not find better identifications by using or not chemical information. This is probably the P15 case, already complete winner at Step 1. This could be also the case of P1, to which was only missing massicot in sample 4. If we had decided to range massicot among the secondary phases, there would have been more winners in this SMRR.

Otherwise results are generally improved as a consequence of the chemistry knowledge. There are two new complete winners (10 identified phases) : P19 (who updated his PDF release from set 47 to set 49) and P26, a new participant

We have one more software in this Step 2 (Traces) and 5 new participants. The mean number of phases identified for each sample is given below (nr = no result provided ; id = incomplete database precluding sample 2 identification), and also the numbers given by the best performer (mixing the software versions) and the worst one. This table can be compared to the equivalent one above, made at Step 1. An improved score if compare to Step 1 is noted in blue (occuring for samples 1 to 4), and a worst score is noted in dark blue (occuring for samples 3 and 4).
 
Software Participants Sample 1 Sample 2 Sample 3 Sample 4
EVA - Socabim/Bruker P5, P9, P11, P12, P13
P16, P17, P22, P26, P28
3.6/4 (+0.27)- 4/4 - 3/4 0.50/1 - 1/1 - 0/1 0.7/1 (-0.05)- 1/1 - 0/1 3.3/4 (+0.38)- 4/4 - 3/4
JADE - MDI P3, P8, P23 4/4 - 4/4 - 4/4 1/1 - 1/1 - 1/1 0.66/1(-0.09) - 1/1 - 0/1 3/4 (-0.25)- 3/4 - 3/4
Highscore - Philips P4, P30 3.5/4 (+0.5)- 4/4 - 3/4 0.5/1 (+0.5) - 1/1 - 0/1 0.5/1 (+0.5) - 1/1 - 0/1 3/4 (-1) - 4/4 - 2/4
Graphics & Identify - Philips P7, P24, P29 2.67/4 - 4/4 - 1/4 0.66/1(+0.66)- 1/1 - 0/1 0.33/1 (-0.33)- 1/1 - 0/1 2.67/4(+0.33)- 3/4 - 2/4
FARHAN P10 3/4 nr nr nr
Bede Search/Match P14 3/4 1/1 (Hanawalt) 0/1 3/4
Yakimov P19 4/4 1/1 (+1 :set 49) 1/1 4/4
CSM - Oxford Cryosystems P20 4/4 1/1 1/1 (+1) 3/4
PHAN P21 4/4  (+1) id 1/1 3/4
TRACES P27 4/4 0/1 1/1 3/4



General conclusion

We are tempted to conclude, owing to the excellent results obtained by some participants at Step 1, without chemistry data, that elemental composition is not absolutely necessary to a powder diffraction expert success in phase identification, even for a mixture of up to 4 phases. However, a sample origin allowing to select a PDF subset (organic, mineral, organometallic...) helps a lot.

The SMRR-2002 shows quite clearly how a good search-match software, in expert hands, combined with an up-to-date PDF can perform efficiently  in solid state phase identification. Of course, this efficiency depends on the PDF completeness, which is not realized yet for organic and organometallic compounds, as shown by the thalidomide case of sample 3, a so sadly famous molecule that it would be better to identify it, whatever the polymorph.


Post-deadline comments from Participants

Send them to any of the email address below, giving your participant number. They will be gathered here.

- Participant 16 discloses his identity :
Emmanuel Garnier, UMR 6503 équipe electrocatalyse, 40 Av du recteur Pineau, 86022 POITIERS CEDEX, France, Email : egarnier@univ-poitiers.fr


J.-M. Le Meins : JM.Le_Meins@univ-mulhouse.fr
L.M.D. Cranswick : l.m.d.cranswick@dl.ac.uk
A. Le Bail : alb@cristal.org

May-June 2002 - Sponsored by the SDPD Internet Course