Re: R: CrySize error in TOPAS

[Łukasz Kruszewski]

Hello Simona. Thank you for the tip. Can you please tell me which refined
parameters did you mean? I suppose you've meant the Sample Corrections and
not the Intstrumental Parameters?

Best regards,

Luke Kruszewski


> Dear Lukasz, dear all:
>
> Before eliminating the contribution of the sample to peak broadening (i.e.
> before suppressing the CS_L instruction), it would be safer to understand
> if the value of 9000 nm is sensible or not. Make sure that there is no
> refined variable, in your input, contributing too much to peak broadening.
> If this variable exists, the high value of the crystal simply tries to
> counterbalance the broadening effect of that variable.
>
> In this respect, I would follow Peter'suggestion to go carefully through
> the correlation matrix provided by Topas when do_errors is at work and
> verify if CS_L strongly correlates with some other variable.
>
> Kind regards,
> Simona
>
> 
> Simona Galli, Prof.
> Dipartimento di Scienza e Alta Tecnologia
> Università dell'Insubria
> Via Valleggio, 9
> 22100 Como - Italy
>
> e-mail: simona.ga...@uninsubria.it
> tel: +39-031-2386627
> url: scienze-como.uninsubria.it/sgalli
>
> Treasurer of the Italian Crystallographic Association
> tesori...@cristallografia.org
> 
>
> - Messaggio originale -
> Da: "Cline, James Dr. (Fed)" <james.cl...@nist.gov>
> Inviato: ‎27/‎07/‎2016 19:17
> A: "rietveld_l@ill.fr" <rietveld_l@ill.fr>
> Cc: ""Łukasz Kruszewski"" <lkruszew...@twarda.pan.pl>
> Oggetto: RE: CrySize error in TOPAS
>
> That means the value is indeterminate with respect to the refinement and
> the contribution of "CrySize" [crystallite size broadening] to the
> observation is nearly zero.  Try turning it off and see what the residuals
> do.
>
> Jim
>
>
> James P. Cline
> Materials Measurement Science Division  
> National Institute of Standards and Technology
> 100 Bureau Dr. stop 8520 [ B113 / Bldg 217 ]
> Gaithersburg, MD 20899-8523    USA
> jcl...@nist.gov
> (301) 975 5793
> FAX (301) 975 5334
>
> -Original Message-
> From: "Łukasz Kruszewski" [mailto:lkruszew...@twarda.pan.pl]
> Sent: Wednesday, July 27, 2016 1:08 PM
> To: Cline, James Dr. (Fed) <james.cl...@nist.gov>
> Cc: rietveld_l@ill.fr; "Łukasz Kruszewski" <lkruszew...@twarda.pan.pl>
> Subject: RE: CrySize error in TOPAS
>
> Hello James. I just read the error that is reported for each refined
> parameter in TOPAS. I obtain value like, e.g., 9000 nm, and the error is,
> e.g., 205006.
>
> Best regards,
>
> Łukasz Kruszewski
>
>
>> By what metric are you determining that the CrySize value is in error?
>>
>>
>> James P. Cline
>> Materials Measurement Science Division National Institute of Standards
>> and Technology
>> 100 Bureau Dr. stop 8520 [ B113 / Bldg 217 ] Gaithersburg, MD
>> 20899-8523    USA jcl...@nist.gov
>> (301) 975 5793
>> FAX (301) 975 5334
>>
>> -Original Message-
>> From: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] On
>> Behalf Of "Lukasz Kruszewski"
>> Sent: Wednesday, July 27, 2016 10:22 AM
>> To: rietveld_l@ill.fr
>> Subject: CrySize error in TOPAS
>>
>> Dera friends,
>>
>> I'm doing Rietveld refinements in TOPAS; I get rather good fit of the
>> reflections, rather good wt.%, but I've observed large errors for the
>> CrySize (Lorentzian) values for some introduced Structures. I've tried
>> to change it by refining CrySize (Gaussian), but it only changed in
>> few particular cases. I'm rather sure that the intrumental parameters
>> (geometry of the diffractometer was analyzed with the use of LaB6, Si,
>> and other standards) and corrections (sample displ. etc.) are OK and I
>> suppose these factors shouldn't influence (?) the CrySize values. I
>> always constrain the minimum (20 starting value) and maximum (1
>> nm) value for CrySize; I usually refine strain, but I've noticed that
>> it doesn't influence the results (at least the wt.% calculated). Rwp,
>> goodness of fit and Durbin-Watson statistics R values are OK; also,
>> the calculated background line is "flat", i.e., there is no mistaking
>> of the background with reflections; the shapes of the reflections in
>> the calculated diffractograms seem to be OK, too. I was thus wondering
>> if these high errors coming from the CrySize are that important for the
>> refinement?
>>
>> Best rega

RE: CrySize error in TOPAS

[Łukasz Kruszewski]

Hi Alan. Thank you for your answer. I will post the list as soon as I get
to the program. I always use FP for Peak Type. I also do not use any
correction for peak tails (i.e., I do not use Tube Tails, as I do not
observe the typical Tube-Tails features).

Best regards,

Luke Kruszewski


> Hi Luke
>
> The weight percents should not differ if CrySize is irrelevant. Can you
> post a list of  the weight percents with and without CyrSize as well as
> Rwp values.
>
> Also, what peak type are using; I hope it's not PVII as it can give
> incorrect results when the exponent is small leading very long peak tails.
> cheers
> alan
>
> -Original Message-
> From: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] On
> Behalf Of "Lukasz Kruszewski"
> Sent: Thursday, July 28, 2016 3:21 AM
> To: Cline, James Dr. (Fed)
> Cc: rietveld_l@ill.fr; "Łukasz Kruszewski"
> Subject: RE: CrySize error in TOPAS
>
> Thank you very much, Jim. I do appreciate this. I though it is not
> "allowed" not to use the CrySize, maybe because I've mixed crystal size
> and crystallite size... However, I did such a single refinement whthout
> any CrySize(s) used. The residuals were OK (that is, not much worse than
> when using the CrySize, that could possibly overparametrize the refinement
> and push it towards the false-correct Rwp etc.), but the wt.% values
> obtained differed quite a lot from the ones obtained when using the
> CrySize. This difference in wt.% a bit worries me, because I'm working
> with TOPAS & Rietveld for some years and I still lack confidence (-;
> Patience matters...
>
> Best regards,
>
> Luke Kruszewski
>
>
>
>> That means the value is indeterminate with respect to the refinement
>> and the contribution of "CrySize" [crystallite size broadening] to the
>> observation is nearly zero.  Try turning it off and see what the
>> residuals do.
>>
>> Jim
>>
>>
>> James P. Cline
>> Materials Measurement Science Division National Institute of Standards
>> and Technology
>> 100 Bureau Dr. stop 8520 [ B113 / Bldg 217 ] Gaithersburg, MD
>> 20899-8523USA jcl...@nist.gov
>> (301) 975 5793
>> FAX (301) 975 5334
>>
>> -Original Message-
>> From: "Łukasz Kruszewski" [mailto:lkruszew...@twarda.pan.pl]
>> Sent: Wednesday, July 27, 2016 1:08 PM
>> To: Cline, James Dr. (Fed) <james.cl...@nist.gov>
>> Cc: rietveld_l@ill.fr; "Łukasz Kruszewski" <lkruszew...@twarda.pan.pl>
>> Subject: RE: CrySize error in TOPAS
>>
>> Hello James. I just read the error that is reported for each refined
>> parameter in TOPAS. I obtain value like, e.g., 9000 nm, and the error
>> is, e.g., 205006.
>>
>> Best regards,
>>
>> Łukasz Kruszewski
>>
>>
>>> By what metric are you determining that the CrySize value is in error?
>>>
>>>
>>> James P. Cline
>>> Materials Measurement Science Division National Institute of
>>> Standards and Technology
>>> 100 Bureau Dr. stop 8520 [ B113 / Bldg 217 ] Gaithersburg, MD
>>> 20899-8523USA jcl...@nist.gov
>>> (301) 975 5793
>>> FAX (301) 975 5334
>>>
>>> -Original Message-
>>> From: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] On
>>> Behalf Of "Lukasz Kruszewski"
>>> Sent: Wednesday, July 27, 2016 10:22 AM
>>> To: rietveld_l@ill.fr
>>> Subject: CrySize error in TOPAS
>>>
>>> Dera friends,
>>>
>>> I'm doing Rietveld refinements in TOPAS; I get rather good fit of the
>>> reflections, rather good wt.%, but I've observed large errors for the
>>> CrySize (Lorentzian) values for some introduced Structures. I've
>>> tried to change it by refining CrySize (Gaussian), but it only
>>> changed in few particular cases. I'm rather sure that the intrumental
>>> parameters (geometry of the diffractometer was analyzed with the use
>>> of LaB6, Si, and other standards) and corrections (sample displ.
>>> etc.) are OK and I suppose these factors shouldn't influence (?) the
>>> CrySize values. I always constrain the minimum (20 starting value)
>>> and maximum (1
>>> nm) value for CrySize; I usually refine strain, but I've noticed that
>>> it doesn't influence the results (at least the wt.% calculated). Rwp,
>>> goodness of fit and Durbin-Watson statistics R values are OK; also,
>>> the calculated background line is "flat", i.e., there is no mistaking
>>> of the background with reflections; the sh

Re: Re[2]: CrySize error in TOPAS

[Łukasz Kruszewski]

Hello Frantisek! Many thanks for this tip. I use v. 4.0.

Best regards,

Łukasz Kruszewski


> Dear Lukasz,
>
> I dont no which version of Topas do you use. Just for your information -
> the current version Topas 5 enables you to calculate the correlation
> matrix
> directly from GUI. Just click on "correlation matrix button" a run
> calculation.
>
> Frantisek Laufek
> Czech Geological Survey
>
>
>
>
>
> - Původní zpráva -
> Odesilatel: "Peter Y. Zavalij" <pzava...@umd.edu>
> Příjemce: "Łukasz Kruszewski" <lkruszew...@twarda.pan.pl>
> Kopie: "Cline, James Dr. (Fed)" <james.cl...@nist.gov>, rietveld_l@ill.fr
> Datum: 2016-07-27 19:23
> Předmět: Re: CrySize error in TOPAS
>
> If you switch from GUI mode to launch mode and perform refinement, you
> will see correlation matrix at the end of .inp file and can tell which
> parameters correlate a lot and figure out what's causing such large error.
> I also think that this error is not strange for such large cryst.size as
> it is basically beyond the limt of the methods.
> Peter
>
>
>
>
> 
> Dr. Peter Y. Zavalij
> Director - X-ray Crystallographic Center
> University of Maryland, College Park, MD 20832
>
> On Wed, Jul 27, 2016 at 1:07 PM, "Łukasz Kruszewski"
> <lkruszew...@twarda.pan.pl> wrote:
> Hello James. I just read the error that is reported for each refined
> parameter in TOPAS. I obtain value like, e.g., 9000 nm, and the error is,
> e.g., 205006.
>
> Best regards,
>
> Łukasz Kruszewski
>
>
>> By what metric are you determining that the CrySize value is in error?
>>
>>
>> James P. Cline
>> Materials Measurement Science Division
>> National Institute of Standards and Technology
>> 100 Bureau Dr. stop 8520 [ B113 / Bldg 217 ]
>> Gaithersburg, MD 20899-8523USA
>> jcl...@nist.gov
>> (301) 975 5793
>> FAX (301) 975 5334
>>
>> -Original Message-
>> From: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] On
>> Behalf Of "Lukasz Kruszewski"
>> Sent: Wednesday, July 27, 2016 10:22 AM
>> To: rietveld_l@ill.fr
>> Subject: CrySize error in TOPAS
>>
>> Dera friends,
>>
>> I'm doing Rietveld refinements in TOPAS; I get rather good fit of the
>> reflections, rather good wt.%, but I've observed large errors for the
>> CrySize (Lorentzian) values for some introduced Structures. I've tried
>> to
>> change it by refining CrySize (Gaussian), but it only changed in few
>> particular cases. I'm rather sure that the intrumental parameters
>> (geometry of the diffractometer was analyzed with the use of LaB6, Si,
>> and
>> other standards) and corrections (sample displ. etc.) are OK and I
>> suppose
>> these factors shouldn't influence (?) the CrySize values. I always
>> constrain the minimum (20 starting value) and maximum (1 nm) value
>> for
>> CrySize; I usually refine strain, but I've noticed that it doesn't
>> influence the results (at least the wt.% calculated). Rwp, goodness of
>> fit
>> and Durbin-Watson statistics R values are OK; also, the calculated
>> background line is "flat", i.e., there is no mistaking of the background
>> with reflections; the shapes of the reflections in the calculated
>> diffractograms seem to be OK, too. I was thus wondering if these high
>> errors coming from the CrySize are that important for the refinement?
>>
>> Best regards,
>>
>>
>> --
>> Łukasz Kruszewski, Ph.D., adjunct
>> Polish Academy of Sciences
>> Institute of Geological Sciences
>> Twarda 51/55 str.
>> 00-818 Warsaw
>> Poland
>>
>
>
> --
> Łukasz Kruszewski, Ph.D., adjunct
> Polish Academy of Sciences
> Institute of Geological Sciences
> Twarda 51/55 str.
> 00-818 Warsaw
> Poland
>
>
> ++
> Please do NOT attach files to the whole list
> <alan.he...@neutronoptics.com>
> Send commands to <lists...@ill.fr> eg: HELP as the subject with no body
> text
> The Rietveld_L list archive is on
> http://www.mail-archive.com/rietveld_l@ill.fr/
> ++
>
>
>
>
>
> ++
> Please do NOT attach files to the whole list
> <alan.he...@neutronoptics.com>
> Send commands to <lists...@ill.fr> eg: HELP as the subject with no body
> text
&

Re[2]: CrySize error in TOPAS

[František Laufek]

Dear Lukasz,

I dont no which version of Topas do you use. Just for your information - the 
current version Topas 5 enables you to calculate the correlation matrix 
directly from GUI. Just click on "correlation matrix button" a run calculation. 

Frantisek Laufek
Czech Geological Survey





- Původní zpráva -
Odesilatel: "Peter Y. Zavalij" <pzava...@umd.edu>
Příjemce: "Łukasz Kruszewski" <lkruszew...@twarda.pan.pl>
Kopie: "Cline, James Dr. (Fed)" <james.cl...@nist.gov>, rietveld_l@ill.fr
Datum: 2016-07-27 19:23
Předmět: Re: CrySize error in TOPAS

If you switch from GUI mode to launch mode and perform refinement, you will see 
correlation matrix at the end of .inp file and can tell which parameters 
correlate a lot and figure out what's causing such large error.
I also think that this error is not strange for such large cryst.size as it is 
basically beyond the limt of the methods.
Peter





Dr. Peter Y. Zavalij
Director - X-ray Crystallographic Center
University of Maryland, College Park, MD 20832

On Wed, Jul 27, 2016 at 1:07 PM, "Łukasz Kruszewski" 
<lkruszew...@twarda.pan.pl> wrote:
Hello James. I just read the error that is reported for each refined
parameter in TOPAS. I obtain value like, e.g., 9000 nm, and the error is,
e.g., 205006.

Best regards,

Łukasz Kruszewski


> By what metric are you determining that the CrySize value is in error?
>
>
> James P. Cline
> Materials Measurement Science Division  
> National Institute of Standards and Technology
> 100 Bureau Dr. stop 8520 [ B113 / Bldg 217 ]
> Gaithersburg, MD 20899-8523USA
> jcl...@nist.gov
> (301) 975 5793
> FAX (301) 975 5334
>
> -Original Message-
> From: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] On
> Behalf Of "Lukasz Kruszewski"
> Sent: Wednesday, July 27, 2016 10:22 AM
> To: rietveld_l@ill.fr
> Subject: CrySize error in TOPAS
>
> Dera friends,
>
> I'm doing Rietveld refinements in TOPAS; I get rather good fit of the
> reflections, rather good wt.%, but I've observed large errors for the
> CrySize (Lorentzian) values for some introduced Structures. I've tried to
> change it by refining CrySize (Gaussian), but it only changed in few
> particular cases. I'm rather sure that the intrumental parameters
> (geometry of the diffractometer was analyzed with the use of LaB6, Si, and
> other standards) and corrections (sample displ. etc.) are OK and I suppose
> these factors shouldn't influence (?) the CrySize values. I always
> constrain the minimum (20 starting value) and maximum (1 nm) value for
> CrySize; I usually refine strain, but I've noticed that it doesn't
> influence the results (at least the wt.% calculated). Rwp, goodness of fit
> and Durbin-Watson statistics R values are OK; also, the calculated
> background line is "flat", i.e., there is no mistaking of the background
> with reflections; the shapes of the reflections in the calculated
> diffractograms seem to be OK, too. I was thus wondering if these high
> errors coming from the CrySize are that important for the refinement?
>
> Best regards,
>
>
> --
> Łukasz Kruszewski, Ph.D., adjunct
> Polish Academy of Sciences
> Institute of Geological Sciences
> Twarda 51/55 str.
> 00-818 Warsaw
> Poland
>


--
Łukasz Kruszewski, Ph.D., adjunct
Polish Academy of Sciences
Institute of Geological Sciences
Twarda 51/55 str.
00-818 Warsaw
Poland


++
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++





++
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++



++
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++

R: CrySize error in TOPAS

[Simona Galli]

Dear Lukasz, dear all:

Before eliminating the contribution of the sample to peak broadening (i.e. 
before suppressing the CS_L instruction), it would be safer to understand if 
the value of 9000 nm is sensible or not. Make sure that there is no refined 
variable, in your input, contributing too much to peak broadening. If this 
variable exists, the high value of the crystal simply tries to counterbalance 
the broadening effect of that variable.

In this respect, I would follow Peter'suggestion to go carefully through the 
correlation matrix provided by Topas when do_errors is at work and verify if 
CS_L strongly correlates with some other variable.

Kind regards,
Simona


Simona Galli, Prof.
Dipartimento di Scienza e Alta Tecnologia
Università dell'Insubria
Via Valleggio, 9
22100 Como - Italy

e-mail: simona.ga...@uninsubria.it
tel: +39-031-2386627
url: scienze-como.uninsubria.it/sgalli

Treasurer of the Italian Crystallographic Association
tesori...@cristallografia.org


- Messaggio originale -
Da: "Cline, James Dr. (Fed)" <james.cl...@nist.gov>
Inviato: ‎27/‎07/‎2016 19:17
A: "rietveld_l@ill.fr" <rietveld_l@ill.fr>
Cc: ""Łukasz Kruszewski"" <lkruszew...@twarda.pan.pl>
Oggetto: RE: CrySize error in TOPAS

That means the value is indeterminate with respect to the refinement and the 
contribution of "CrySize" [crystallite size broadening] to the observation is 
nearly zero.  Try turning it off and see what the residuals do.

Jim


James P. Cline
Materials Measurement Science Division  
National Institute of Standards and Technology
100 Bureau Dr. stop 8520 [ B113 / Bldg 217 ]
Gaithersburg, MD 20899-8523    USA
jcl...@nist.gov
(301) 975 5793
FAX (301) 975 5334

-Original Message-
From: "Łukasz Kruszewski" [mailto:lkruszew...@twarda.pan.pl] 
Sent: Wednesday, July 27, 2016 1:08 PM
To: Cline, James Dr. (Fed) <james.cl...@nist.gov>
Cc: rietveld_l@ill.fr; "Łukasz Kruszewski" <lkruszew...@twarda.pan.pl>
Subject: RE: CrySize error in TOPAS

Hello James. I just read the error that is reported for each refined parameter 
in TOPAS. I obtain value like, e.g., 9000 nm, and the error is, e.g., 205006.

Best regards,

Łukasz Kruszewski


> By what metric are you determining that the CrySize value is in error?
>
>
> James P. Cline
> Materials Measurement Science Division National Institute of Standards 
> and Technology
> 100 Bureau Dr. stop 8520 [ B113 / Bldg 217 ] Gaithersburg, MD 
> 20899-8523    USA jcl...@nist.gov
> (301) 975 5793
> FAX (301) 975 5334
>
> -Original Message-
> From: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] On 
> Behalf Of "Lukasz Kruszewski"
> Sent: Wednesday, July 27, 2016 10:22 AM
> To: rietveld_l@ill.fr
> Subject: CrySize error in TOPAS
>
> Dera friends,
>
> I'm doing Rietveld refinements in TOPAS; I get rather good fit of the 
> reflections, rather good wt.%, but I've observed large errors for the 
> CrySize (Lorentzian) values for some introduced Structures. I've tried 
> to change it by refining CrySize (Gaussian), but it only changed in 
> few particular cases. I'm rather sure that the intrumental parameters 
> (geometry of the diffractometer was analyzed with the use of LaB6, Si, 
> and other standards) and corrections (sample displ. etc.) are OK and I 
> suppose these factors shouldn't influence (?) the CrySize values. I 
> always constrain the minimum (20 starting value) and maximum (1 
> nm) value for CrySize; I usually refine strain, but I've noticed that 
> it doesn't influence the results (at least the wt.% calculated). Rwp, 
> goodness of fit and Durbin-Watson statistics R values are OK; also, 
> the calculated background line is "flat", i.e., there is no mistaking 
> of the background with reflections; the shapes of the reflections in 
> the calculated diffractograms seem to be OK, too. I was thus wondering 
> if these high errors coming from the CrySize are that important for the 
> refinement?
>
> Best regards,
>
>
> --
> Łukasz Kruszewski, Ph.D., adjunct
> Polish Academy of Sciences
> Institute of Geological Sciences
> Twarda 51/55 str.
> 00-818 Warsaw
> Poland
>


--
Łukasz Kruszewski, Ph.D., adjunct
Polish Academy of Sciences
Institute of Geological Sciences
Twarda 51/55 str.
00-818 Warsaw
Poland
++
Please do NOT attach files to the whole list <alan.he...@neutronoptics.com>
Send commands to <lists...@ill.fr> eg: HELP as the subject with no body text
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++

Re: CrySize error in TOPAS

[Łukasz Kruszewski]

Hello Peter. Thank you very much. I will do so and check it. I find this
mailing list very useful - a lot of useful informations from kind people
that like to share - thank you!

Best regards,

Łukasz Kruszewski


> If you switch from GUI mode to launch mode and perform refinement, you
> will
> see correlation matrix at the end of .inp file and can tell which
> parameters correlate a lot and figure out what's causing such large error.
> I also think that this error is not strange for such large cryst.size as
> it
> is basically beyond the limt of the methods.
> Peter
>
> 
> Dr. Peter Y. Zavalij
> Director - X-ray Crystallographic Center
> University of Maryland, College Park, MD 20832
>
> On Wed, Jul 27, 2016 at 1:07 PM, "Łukasz Kruszewski" <
> lkruszew...@twarda.pan.pl> wrote:
>
>> Hello James. I just read the error that is reported for each refined
>> parameter in TOPAS. I obtain value like, e.g., 9000 nm, and the error
>> is,
>> e.g., 205006.
>>
>> Best regards,
>>
>> Łukasz Kruszewski
>>
>>
>> > By what metric are you determining that the CrySize value is in error?
>> >
>> >
>> > James P. Cline
>> > Materials Measurement Science Division
>> > National Institute of Standards and Technology
>> > 100 Bureau Dr. stop 8520 [ B113 / Bldg 217 ]
>> > Gaithersburg, MD 20899-8523USA
>> > jcl...@nist.gov
>> > (301) 975 5793
>> > FAX (301) 975 5334
>> >
>> > -Original Message-
>> > From: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] On
>> > Behalf Of "Lukasz Kruszewski"
>> > Sent: Wednesday, July 27, 2016 10:22 AM
>> > To: rietveld_l@ill.fr
>> > Subject: CrySize error in TOPAS
>> >
>> > Dera friends,
>> >
>> > I'm doing Rietveld refinements in TOPAS; I get rather good fit of the
>> > reflections, rather good wt.%, but I've observed large errors for the
>> > CrySize (Lorentzian) values for some introduced Structures. I've tried
>> to
>> > change it by refining CrySize (Gaussian), but it only changed in few
>> > particular cases. I'm rather sure that the intrumental parameters
>> > (geometry of the diffractometer was analyzed with the use of LaB6, Si,
>> and
>> > other standards) and corrections (sample displ. etc.) are OK and I
>> suppose
>> > these factors shouldn't influence (?) the CrySize values. I always
>> > constrain the minimum (20 starting value) and maximum (1 nm) value
>> for
>> > CrySize; I usually refine strain, but I've noticed that it doesn't
>> > influence the results (at least the wt.% calculated). Rwp, goodness of
>> fit
>> > and Durbin-Watson statistics R values are OK; also, the calculated
>> > background line is "flat", i.e., there is no mistaking of the
>> background
>> > with reflections; the shapes of the reflections in the calculated
>> > diffractograms seem to be OK, too. I was thus wondering if these high
>> > errors coming from the CrySize are that important for the refinement?
>> >
>> > Best regards,
>> >
>> >
>> > --
>> > Łukasz Kruszewski, Ph.D., adjunct
>> > Polish Academy of Sciences
>> > Institute of Geological Sciences
>> > Twarda 51/55 str.
>> > 00-818 Warsaw
>> > Poland
>> >
>>
>>
>> --
>> Łukasz Kruszewski, Ph.D., adjunct
>> Polish Academy of Sciences
>> Institute of Geological Sciences
>> Twarda 51/55 str.
>> 00-818 Warsaw
>> Poland
>>
>> ++
>> Please do NOT attach files to the whole list
>> <alan.he...@neutronoptics.com
>> >
>> Send commands to <lists...@ill.fr> eg: HELP as the subject with no body
>> text
>> The Rietveld_L list archive is on
>> http://www.mail-archive.com/rietveld_l@ill.fr/
>> ++
>>
>>
>>
> ++
> Please do NOT attach files to the whole list
> <alan.he...@neutronoptics.com>
> Send commands to <lists...@ill.fr> eg: HELP as the subject with no body
> text
> The Rietveld_L list archive is on
> http://www.mail-archive.com/rietveld_l@ill.fr/
> ++
>
>


-- 
Łukasz Kruszewski, Ph.D., adjunct
Polish Academy of Sciences
Institute of Geological Sciences
Twarda 51/55 str.
00-818 Warsaw
Poland
++
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++

RE: CrySize error in TOPAS

[Alan Coelho]

Hi Luke

The weight percents should not differ if CrySize is irrelevant. Can you post a 
list of  the weight percents with and without CyrSize as well as Rwp values. 

Also, what peak type are using; I hope it's not PVII as it can give incorrect 
results when the exponent is small leading very long peak tails.
cheers
alan

-Original Message-
From: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] On Behalf Of 
"Lukasz Kruszewski"
Sent: Thursday, July 28, 2016 3:21 AM
To: Cline, James Dr. (Fed)
Cc: rietveld_l@ill.fr; "Łukasz Kruszewski"
Subject: RE: CrySize error in TOPAS

Thank you very much, Jim. I do appreciate this. I though it is not "allowed" 
not to use the CrySize, maybe because I've mixed crystal size and crystallite 
size... However, I did such a single refinement whthout any CrySize(s) used. 
The residuals were OK (that is, not much worse than when using the CrySize, 
that could possibly overparametrize the refinement and push it towards the 
false-correct Rwp etc.), but the wt.% values obtained differed quite a lot from 
the ones obtained when using the CrySize. This difference in wt.% a bit worries 
me, because I'm working with TOPAS & Rietveld for some years and I still lack 
confidence (-; Patience matters...

Best regards,

Luke Kruszewski



> That means the value is indeterminate with respect to the refinement 
> and the contribution of "CrySize" [crystallite size broadening] to the 
> observation is nearly zero.  Try turning it off and see what the 
> residuals do.
>
> Jim
>
>
> James P. Cline
> Materials Measurement Science Division National Institute of Standards 
> and Technology
> 100 Bureau Dr. stop 8520 [ B113 / Bldg 217 ] Gaithersburg, MD 
> 20899-8523USA jcl...@nist.gov
> (301) 975 5793
> FAX (301) 975 5334
>
> -Original Message-
> From: "Łukasz Kruszewski" [mailto:lkruszew...@twarda.pan.pl]
> Sent: Wednesday, July 27, 2016 1:08 PM
> To: Cline, James Dr. (Fed) <james.cl...@nist.gov>
> Cc: rietveld_l@ill.fr; "Łukasz Kruszewski" <lkruszew...@twarda.pan.pl>
> Subject: RE: CrySize error in TOPAS
>
> Hello James. I just read the error that is reported for each refined 
> parameter in TOPAS. I obtain value like, e.g., 9000 nm, and the error 
> is, e.g., 205006.
>
> Best regards,
>
> Łukasz Kruszewski
>
>
>> By what metric are you determining that the CrySize value is in error?
>>
>>
>> James P. Cline
>> Materials Measurement Science Division National Institute of 
>> Standards and Technology
>> 100 Bureau Dr. stop 8520 [ B113 / Bldg 217 ] Gaithersburg, MD
>> 20899-8523USA jcl...@nist.gov
>> (301) 975 5793
>> FAX (301) 975 5334
>>
>> -Original Message-
>> From: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] On 
>> Behalf Of "Lukasz Kruszewski"
>> Sent: Wednesday, July 27, 2016 10:22 AM
>> To: rietveld_l@ill.fr
>> Subject: CrySize error in TOPAS
>>
>> Dera friends,
>>
>> I'm doing Rietveld refinements in TOPAS; I get rather good fit of the 
>> reflections, rather good wt.%, but I've observed large errors for the 
>> CrySize (Lorentzian) values for some introduced Structures. I've 
>> tried to change it by refining CrySize (Gaussian), but it only 
>> changed in few particular cases. I'm rather sure that the intrumental 
>> parameters (geometry of the diffractometer was analyzed with the use 
>> of LaB6, Si, and other standards) and corrections (sample displ. 
>> etc.) are OK and I suppose these factors shouldn't influence (?) the 
>> CrySize values. I always constrain the minimum (20 starting value) 
>> and maximum (1
>> nm) value for CrySize; I usually refine strain, but I've noticed that 
>> it doesn't influence the results (at least the wt.% calculated). Rwp, 
>> goodness of fit and Durbin-Watson statistics R values are OK; also, 
>> the calculated background line is "flat", i.e., there is no mistaking 
>> of the background with reflections; the shapes of the reflections in 
>> the calculated diffractograms seem to be OK, too. I was thus 
>> wondering if these high errors coming from the CrySize are that 
>> important for the refinement?
>>
>> Best regards,
>>
>>
>> --
>> Łukasz Kruszewski, Ph.D., adjunct
>> Polish Academy of Sciences
>> Institute of Geological Sciences
>> Twarda 51/55 str.
>> 00-818 Warsaw
>> Poland
>>
>
>
> --
> Łukasz Kruszewski, Ph.D., adjunct
> Polish Academy of Sciences
> Institute of Geological Sciences
> Twarda 51/55 str.
> 00-818 Warsaw
> Poland
>


--
Łukasz Kruszewski, Ph.D., adjunct
Polish Academy of Sciences
Institute of Geological Sciences
Twarda 51/55 str.
00-818 Warsaw
Poland

++
Please do NOT attach files to the whole list <alan.he...@neutronoptics.com>
Send commands to <lists...@ill.fr> eg: HELP as the subject with no body text
The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++

RE: CrySize error in TOPAS

[Łukasz Kruszewski]

Thank you very much, Jim. I do appreciate this. I though it is not
"allowed" not to use the CrySize, maybe because I've mixed crystal size
and crystallite size... However, I did such a single refinement whthout
any CrySize(s) used. The residuals were OK (that is, not much worse than
when using the CrySize, that could possibly overparametrize the refinement
and push it towards the false-correct Rwp etc.), but the wt.% values
obtained differed quite a lot from the ones obtained when using the
CrySize. This difference in wt.% a bit worries me, because I'm working
with TOPAS & Rietveld for some years and I still lack confidence (-;
Patience matters...

Best regards,

Luke Kruszewski



> That means the value is indeterminate with respect to the refinement and
> the contribution of "CrySize" [crystallite size broadening] to the
> observation is nearly zero.  Try turning it off and see what the residuals
> do.
>
> Jim
>
>
> James P. Cline
> Materials Measurement Science Division  
> National Institute of Standards and Technology
> 100 Bureau Dr. stop 8520 [ B113 / Bldg 217 ]
> Gaithersburg, MD 20899-8523    USA
> jcl...@nist.gov
> (301) 975 5793
> FAX (301) 975 5334
>
> -Original Message-
> From: "Łukasz Kruszewski" [mailto:lkruszew...@twarda.pan.pl]
> Sent: Wednesday, July 27, 2016 1:08 PM
> To: Cline, James Dr. (Fed) <james.cl...@nist.gov>
> Cc: rietveld_l@ill.fr; "Łukasz Kruszewski" <lkruszew...@twarda.pan.pl>
> Subject: RE: CrySize error in TOPAS
>
> Hello James. I just read the error that is reported for each refined
> parameter in TOPAS. I obtain value like, e.g., 9000 nm, and the error is,
> e.g., 205006.
>
> Best regards,
>
> Łukasz Kruszewski
>
>
>> By what metric are you determining that the CrySize value is in error?
>>
>>
>> James P. Cline
>> Materials Measurement Science Division National Institute of Standards
>> and Technology
>> 100 Bureau Dr. stop 8520 [ B113 / Bldg 217 ] Gaithersburg, MD
>> 20899-8523    USA jcl...@nist.gov
>> (301) 975 5793
>> FAX (301) 975 5334
>>
>> -----Original Message-
>> From: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] On
>> Behalf Of "Lukasz Kruszewski"
>> Sent: Wednesday, July 27, 2016 10:22 AM
>> To: rietveld_l@ill.fr
>> Subject: CrySize error in TOPAS
>>
>> Dera friends,
>>
>> I'm doing Rietveld refinements in TOPAS; I get rather good fit of the
>> reflections, rather good wt.%, but I've observed large errors for the
>> CrySize (Lorentzian) values for some introduced Structures. I've tried
>> to change it by refining CrySize (Gaussian), but it only changed in
>> few particular cases. I'm rather sure that the intrumental parameters
>> (geometry of the diffractometer was analyzed with the use of LaB6, Si,
>> and other standards) and corrections (sample displ. etc.) are OK and I
>> suppose these factors shouldn't influence (?) the CrySize values. I
>> always constrain the minimum (20 starting value) and maximum (1
>> nm) value for CrySize; I usually refine strain, but I've noticed that
>> it doesn't influence the results (at least the wt.% calculated). Rwp,
>> goodness of fit and Durbin-Watson statistics R values are OK; also,
>> the calculated background line is "flat", i.e., there is no mistaking
>> of the background with reflections; the shapes of the reflections in
>> the calculated diffractograms seem to be OK, too. I was thus wondering
>> if these high errors coming from the CrySize are that important for the
>> refinement?
>>
>> Best regards,
>>
>>
>> --
>> Łukasz Kruszewski, Ph.D., adjunct
>> Polish Academy of Sciences
>> Institute of Geological Sciences
>> Twarda 51/55 str.
>> 00-818 Warsaw
>> Poland
>>
>
>
> --
> Łukasz Kruszewski, Ph.D., adjunct
> Polish Academy of Sciences
> Institute of Geological Sciences
> Twarda 51/55 str.
> 00-818 Warsaw
> Poland
>


-- 
Łukasz Kruszewski, Ph.D., adjunct
Polish Academy of Sciences
Institute of Geological Sciences
Twarda 51/55 str.
00-818 Warsaw
Poland
++
Please do NOT attach files to the whole list <alan.he...@neutronoptics.com>
Send commands to <lists...@ill.fr> eg: HELP as the subject with no body text
The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++

RE: CrySize error in TOPAS

[Łukasz Kruszewski]

Thank you very much, Jim. I do appreciate this. I though it is not
"allowed" not to use the CrySize, maybe because I've mixed crystal size
and crystallite size... However, I did such a single refinement whthout
any CrySize(s) used. The residuals were OK (that is, not much worse than
when using the CrySize, that could possibly overparametrize the refinement
and push it towards the false-correct Rwp etc.), but the wt.% values
obtained differed quite a lot from the ones obtained when using the
CrySize. This difference in wt.% a bit worries me, because I'm working
with TOPAS & Rietveld for some years and I still lack confidence (-;
Patience matters...

Best regards,

Luke Kruszewski



> That means the value is indeterminate with respect to the refinement and
> the contribution of "CrySize" [crystallite size broadening] to the
> observation is nearly zero.  Try turning it off and see what the residuals
> do.
>
> Jim
>
>
> James P. Cline
> Materials Measurement Science Division  
> National Institute of Standards and Technology
> 100 Bureau Dr. stop 8520 [ B113 / Bldg 217 ]
> Gaithersburg, MD 20899-8523    USA
> jcl...@nist.gov
> (301) 975 5793
> FAX (301) 975 5334
>
> -Original Message-
> From: "Łukasz Kruszewski" [mailto:lkruszew...@twarda.pan.pl]
> Sent: Wednesday, July 27, 2016 1:08 PM
> To: Cline, James Dr. (Fed) <james.cl...@nist.gov>
> Cc: rietveld_l@ill.fr; "Łukasz Kruszewski" <lkruszew...@twarda.pan.pl>
> Subject: RE: CrySize error in TOPAS
>
> Hello James. I just read the error that is reported for each refined
> parameter in TOPAS. I obtain value like, e.g., 9000 nm, and the error is,
> e.g., 205006.
>
> Best regards,
>
> Łukasz Kruszewski
>
>
>> By what metric are you determining that the CrySize value is in error?
>>
>>
>> James P. Cline
>> Materials Measurement Science Division National Institute of Standards
>> and Technology
>> 100 Bureau Dr. stop 8520 [ B113 / Bldg 217 ] Gaithersburg, MD
>> 20899-8523    USA jcl...@nist.gov
>> (301) 975 5793
>> FAX (301) 975 5334
>>
>> -----Original Message-
>> From: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] On
>> Behalf Of "Lukasz Kruszewski"
>> Sent: Wednesday, July 27, 2016 10:22 AM
>> To: rietveld_l@ill.fr
>> Subject: CrySize error in TOPAS
>>
>> Dera friends,
>>
>> I'm doing Rietveld refinements in TOPAS; I get rather good fit of the
>> reflections, rather good wt.%, but I've observed large errors for the
>> CrySize (Lorentzian) values for some introduced Structures. I've tried
>> to change it by refining CrySize (Gaussian), but it only changed in
>> few particular cases. I'm rather sure that the intrumental parameters
>> (geometry of the diffractometer was analyzed with the use of LaB6, Si,
>> and other standards) and corrections (sample displ. etc.) are OK and I
>> suppose these factors shouldn't influence (?) the CrySize values. I
>> always constrain the minimum (20 starting value) and maximum (1
>> nm) value for CrySize; I usually refine strain, but I've noticed that
>> it doesn't influence the results (at least the wt.% calculated). Rwp,
>> goodness of fit and Durbin-Watson statistics R values are OK; also,
>> the calculated background line is "flat", i.e., there is no mistaking
>> of the background with reflections; the shapes of the reflections in
>> the calculated diffractograms seem to be OK, too. I was thus wondering
>> if these high errors coming from the CrySize are that important for the
>> refinement?
>>
>> Best regards,
>>
>>
>> --
>> Łukasz Kruszewski, Ph.D., adjunct
>> Polish Academy of Sciences
>> Institute of Geological Sciences
>> Twarda 51/55 str.
>> 00-818 Warsaw
>> Poland
>>
>
>
> --
> Łukasz Kruszewski, Ph.D., adjunct
> Polish Academy of Sciences
> Institute of Geological Sciences
> Twarda 51/55 str.
> 00-818 Warsaw
> Poland
>


-- 
Łukasz Kruszewski, Ph.D., adjunct
Polish Academy of Sciences
Institute of Geological Sciences
Twarda 51/55 str.
00-818 Warsaw
Poland
++
Please do NOT attach files to the whole list <alan.he...@neutronoptics.com>
Send commands to <lists...@ill.fr> eg: HELP as the subject with no body text
The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++

Re: CrySize error in TOPAS

[Peter Y. Zavalij]

If you switch from GUI mode to launch mode and perform refinement, you will
see correlation matrix at the end of .inp file and can tell which
parameters correlate a lot and figure out what's causing such large error.
I also think that this error is not strange for such large cryst.size as it
is basically beyond the limt of the methods.
Peter


Dr. Peter Y. Zavalij
Director - X-ray Crystallographic Center
University of Maryland, College Park, MD 20832

On Wed, Jul 27, 2016 at 1:07 PM, "Łukasz Kruszewski" <
lkruszew...@twarda.pan.pl> wrote:

> Hello James. I just read the error that is reported for each refined
> parameter in TOPAS. I obtain value like, e.g., 9000 nm, and the error is,
> e.g., 205006.
>
> Best regards,
>
> Łukasz Kruszewski
>
>
> > By what metric are you determining that the CrySize value is in error?
> >
> >
> > James P. Cline
> > Materials Measurement Science Division
> > National Institute of Standards and Technology
> > 100 Bureau Dr. stop 8520 [ B113 / Bldg 217 ]
> > Gaithersburg, MD 20899-8523USA
> > jcl...@nist.gov
> > (301) 975 5793
> > FAX (301) 975 5334
> >
> > -Original Message-
> > From: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] On
> > Behalf Of "Lukasz Kruszewski"
> > Sent: Wednesday, July 27, 2016 10:22 AM
> > To: rietveld_l@ill.fr
> > Subject: CrySize error in TOPAS
> >
> > Dera friends,
> >
> > I'm doing Rietveld refinements in TOPAS; I get rather good fit of the
> > reflections, rather good wt.%, but I've observed large errors for the
> > CrySize (Lorentzian) values for some introduced Structures. I've tried to
> > change it by refining CrySize (Gaussian), but it only changed in few
> > particular cases. I'm rather sure that the intrumental parameters
> > (geometry of the diffractometer was analyzed with the use of LaB6, Si,
> and
> > other standards) and corrections (sample displ. etc.) are OK and I
> suppose
> > these factors shouldn't influence (?) the CrySize values. I always
> > constrain the minimum (20 starting value) and maximum (1 nm) value
> for
> > CrySize; I usually refine strain, but I've noticed that it doesn't
> > influence the results (at least the wt.% calculated). Rwp, goodness of
> fit
> > and Durbin-Watson statistics R values are OK; also, the calculated
> > background line is "flat", i.e., there is no mistaking of the background
> > with reflections; the shapes of the reflections in the calculated
> > diffractograms seem to be OK, too. I was thus wondering if these high
> > errors coming from the CrySize are that important for the refinement?
> >
> > Best regards,
> >
> >
> > --
> > Łukasz Kruszewski, Ph.D., adjunct
> > Polish Academy of Sciences
> > Institute of Geological Sciences
> > Twarda 51/55 str.
> > 00-818 Warsaw
> > Poland
> >
>
>
> --
> Łukasz Kruszewski, Ph.D., adjunct
> Polish Academy of Sciences
> Institute of Geological Sciences
> Twarda 51/55 str.
> 00-818 Warsaw
> Poland
>
> ++
> Please do NOT attach files to the whole list <alan.he...@neutronoptics.com
> >
> Send commands to <lists...@ill.fr> eg: HELP as the subject with no body
> text
> The Rietveld_L list archive is on
> http://www.mail-archive.com/rietveld_l@ill.fr/
> ++
>
>
>
++
Please do NOT attach files to the whole list <alan.he...@neutronoptics.com>
Send commands to <lists...@ill.fr> eg: HELP as the subject with no body text
The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++

RE: CrySize error in TOPAS

[Łukasz Kruszewski]

Thank you very much, Jim. I do appreciate this. I though it is not
"allowed" not to use the CrySize, maybe because I've mixed crystal size
and crystallite size... However, I did such a single refinement whthout
any CrySize(s) used. The residuals were OK (that is, not much worse than
when using the CrySize, that could possibly overparametrize the refinement
and push it towards the false-correct Rwp etc.), but the wt.% values
obtained differed quite a lot from the ones obtained when using the
CrySize. This difference in wt.% a bit worries me, because I'm working
with TOPAS & Rietveld for some years and I still lack confidence (-;
Patience matters...

Best regards,

Luke Kruszewski



> That means the value is indeterminate with respect to the refinement and
> the contribution of "CrySize" [crystallite size broadening] to the
> observation is nearly zero.  Try turning it off and see what the residuals
> do.
>
> Jim
>
>
> James P. Cline
> Materials Measurement Science Division  
> National Institute of Standards and Technology
> 100 Bureau Dr. stop 8520 [ B113 / Bldg 217 ]
> Gaithersburg, MD 20899-8523    USA
> jcl...@nist.gov
> (301) 975 5793
> FAX (301) 975 5334
>
> -Original Message-
> From: "Łukasz Kruszewski" [mailto:lkruszew...@twarda.pan.pl]
> Sent: Wednesday, July 27, 2016 1:08 PM
> To: Cline, James Dr. (Fed) <james.cl...@nist.gov>
> Cc: rietveld_l@ill.fr; "Łukasz Kruszewski" <lkruszew...@twarda.pan.pl>
> Subject: RE: CrySize error in TOPAS
>
> Hello James. I just read the error that is reported for each refined
> parameter in TOPAS. I obtain value like, e.g., 9000 nm, and the error is,
> e.g., 205006.
>
> Best regards,
>
> Łukasz Kruszewski
>
>
>> By what metric are you determining that the CrySize value is in error?
>>
>>
>> James P. Cline
>> Materials Measurement Science Division National Institute of Standards
>> and Technology
>> 100 Bureau Dr. stop 8520 [ B113 / Bldg 217 ] Gaithersburg, MD
>> 20899-8523    USA jcl...@nist.gov
>> (301) 975 5793
>> FAX (301) 975 5334
>>
>> -----Original Message-
>> From: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] On
>> Behalf Of "Lukasz Kruszewski"
>> Sent: Wednesday, July 27, 2016 10:22 AM
>> To: rietveld_l@ill.fr
>> Subject: CrySize error in TOPAS
>>
>> Dera friends,
>>
>> I'm doing Rietveld refinements in TOPAS; I get rather good fit of the
>> reflections, rather good wt.%, but I've observed large errors for the
>> CrySize (Lorentzian) values for some introduced Structures. I've tried
>> to change it by refining CrySize (Gaussian), but it only changed in
>> few particular cases. I'm rather sure that the intrumental parameters
>> (geometry of the diffractometer was analyzed with the use of LaB6, Si,
>> and other standards) and corrections (sample displ. etc.) are OK and I
>> suppose these factors shouldn't influence (?) the CrySize values. I
>> always constrain the minimum (20 starting value) and maximum (1
>> nm) value for CrySize; I usually refine strain, but I've noticed that
>> it doesn't influence the results (at least the wt.% calculated). Rwp,
>> goodness of fit and Durbin-Watson statistics R values are OK; also,
>> the calculated background line is "flat", i.e., there is no mistaking
>> of the background with reflections; the shapes of the reflections in
>> the calculated diffractograms seem to be OK, too. I was thus wondering
>> if these high errors coming from the CrySize are that important for the
>> refinement?
>>
>> Best regards,
>>
>>
>> --
>> Łukasz Kruszewski, Ph.D., adjunct
>> Polish Academy of Sciences
>> Institute of Geological Sciences
>> Twarda 51/55 str.
>> 00-818 Warsaw
>> Poland
>>
>
>
> --
> Łukasz Kruszewski, Ph.D., adjunct
> Polish Academy of Sciences
> Institute of Geological Sciences
> Twarda 51/55 str.
> 00-818 Warsaw
> Poland
>


-- 
Łukasz Kruszewski, Ph.D., adjunct
Polish Academy of Sciences
Institute of Geological Sciences
Twarda 51/55 str.
00-818 Warsaw
Poland
++
Please do NOT attach files to the whole list <alan.he...@neutronoptics.com>
Send commands to <lists...@ill.fr> eg: HELP as the subject with no body text
The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++

RE: CrySize error in TOPAS

[Cline, James Dr. (Fed)]

That means the value is indeterminate with respect to the refinement and the 
contribution of "CrySize" [crystallite size broadening] to the observation is 
nearly zero.  Try turning it off and see what the residuals do.

Jim


James P. Cline
Materials Measurement Science Division  
National Institute of Standards and Technology
100 Bureau Dr. stop 8520 [ B113 / Bldg 217 ]
Gaithersburg, MD 20899-8523    USA
jcl...@nist.gov
(301) 975 5793
FAX (301) 975 5334

-Original Message-
From: "Łukasz Kruszewski" [mailto:lkruszew...@twarda.pan.pl] 
Sent: Wednesday, July 27, 2016 1:08 PM
To: Cline, James Dr. (Fed) <james.cl...@nist.gov>
Cc: rietveld_l@ill.fr; "Łukasz Kruszewski" <lkruszew...@twarda.pan.pl>
Subject: RE: CrySize error in TOPAS

Hello James. I just read the error that is reported for each refined parameter 
in TOPAS. I obtain value like, e.g., 9000 nm, and the error is, e.g., 205006.

Best regards,

Łukasz Kruszewski


> By what metric are you determining that the CrySize value is in error?
>
>
> James P. Cline
> Materials Measurement Science Division National Institute of Standards 
> and Technology
> 100 Bureau Dr. stop 8520 [ B113 / Bldg 217 ] Gaithersburg, MD 
> 20899-8523    USA jcl...@nist.gov
> (301) 975 5793
> FAX (301) 975 5334
>
> -Original Message-
> From: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] On 
> Behalf Of "Lukasz Kruszewski"
> Sent: Wednesday, July 27, 2016 10:22 AM
> To: rietveld_l@ill.fr
> Subject: CrySize error in TOPAS
>
> Dera friends,
>
> I'm doing Rietveld refinements in TOPAS; I get rather good fit of the 
> reflections, rather good wt.%, but I've observed large errors for the 
> CrySize (Lorentzian) values for some introduced Structures. I've tried 
> to change it by refining CrySize (Gaussian), but it only changed in 
> few particular cases. I'm rather sure that the intrumental parameters 
> (geometry of the diffractometer was analyzed with the use of LaB6, Si, 
> and other standards) and corrections (sample displ. etc.) are OK and I 
> suppose these factors shouldn't influence (?) the CrySize values. I 
> always constrain the minimum (20 starting value) and maximum (1 
> nm) value for CrySize; I usually refine strain, but I've noticed that 
> it doesn't influence the results (at least the wt.% calculated). Rwp, 
> goodness of fit and Durbin-Watson statistics R values are OK; also, 
> the calculated background line is "flat", i.e., there is no mistaking 
> of the background with reflections; the shapes of the reflections in 
> the calculated diffractograms seem to be OK, too. I was thus wondering 
> if these high errors coming from the CrySize are that important for the 
> refinement?
>
> Best regards,
>
>
> --
> Łukasz Kruszewski, Ph.D., adjunct
> Polish Academy of Sciences
> Institute of Geological Sciences
> Twarda 51/55 str.
> 00-818 Warsaw
> Poland
>


--
Łukasz Kruszewski, Ph.D., adjunct
Polish Academy of Sciences
Institute of Geological Sciences
Twarda 51/55 str.
00-818 Warsaw
Poland
++
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Re: CrySize error in TOPAS

[Łukasz Kruszewski]

Hello Saul. Thank you for your reply. I've meant the calculated
statistical error, that is calculated for each refined parameter in TOPAS;
the values themselves seem to be correct, i.e., they are in the limits
described as <20, 1>.

Best regards,

Łukasz Kruszewski


> Also do you mean error (as in correct value) or calculated statistical
> uncertainty?
>
> Saul
>
> On Wed, Jul 27, 2016 at 9:22 AM, "Łukasz Kruszewski"
>  wrote:
>> Dera friends,
>>
>> I'm doing Rietveld refinements in TOPAS; I get rather good fit of the
>> reflections, rather good wt.%, but I've observed large errors for the
>> CrySize (Lorentzian) values for some introduced Structures. I've tried
>> to
>> change it by refining CrySize (Gaussian), but it only changed in few
>> particular cases. I'm rather sure that the intrumental parameters
>> (geometry of the diffractometer was analyzed with the use of LaB6, Si,
>> and
>> other standards) and corrections (sample displ. etc.) are OK and I
>> suppose
>> these factors shouldn't influence (?) the CrySize values. I always
>> constrain the minimum (20 starting value) and maximum (1 nm) value
>> for
>> CrySize; I usually refine strain, but I've noticed that it doesn't
>> influence the results (at least the wt.% calculated). Rwp, goodness of
>> fit
>> and Durbin-Watson statistics R values are OK; also, the calculated
>> background line is "flat", i.e., there is no mistaking of the background
>> with reflections; the shapes of the reflections in the calculated
>> diffractograms seem to be OK, too. I was thus wondering if these high
>> errors coming from the CrySize are that important for the refinement?
>>
>> Best regards,
>>
>>
>> --
>> Łukasz Kruszewski, Ph.D., adjunct
>> Polish Academy of Sciences
>> Institute of Geological Sciences
>> Twarda 51/55 str.
>> 00-818 Warsaw
>> Poland
>>
>> ++
>> Please do NOT attach files to the whole list
>> 
>> Send commands to  eg: HELP as the subject with no body
>> text
>> The Rietveld_L list archive is on
>> http://www.mail-archive.com/rietveld_l@ill.fr/
>> ++
>>
>>
> ++
> Please do NOT attach files to the whole list
> 
> Send commands to  eg: HELP as the subject with no body
> text
> The Rietveld_L list archive is on
> http://www.mail-archive.com/rietveld_l@ill.fr/
> ++
>
>


-- 
Łukasz Kruszewski, Ph.D., adjunct
Polish Academy of Sciences
Institute of Geological Sciences
Twarda 51/55 str.
00-818 Warsaw
Poland
++
Please do NOT attach files to the whole list 
Send commands to  eg: HELP as the subject with no body text
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++

RE: CrySize error in TOPAS

[Łukasz Kruszewski]

Hello James. I just read the error that is reported for each refined
parameter in TOPAS. I obtain value like, e.g., 9000 nm, and the error is,
e.g., 205006.

Best regards,

Łukasz Kruszewski


> By what metric are you determining that the CrySize value is in error?
>
>
> James P. Cline
> Materials Measurement Science Division  
> National Institute of Standards and Technology
> 100 Bureau Dr. stop 8520 [ B113 / Bldg 217 ]
> Gaithersburg, MD 20899-8523    USA
> jcl...@nist.gov
> (301) 975 5793
> FAX (301) 975 5334
>
> -Original Message-
> From: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] On
> Behalf Of "Lukasz Kruszewski"
> Sent: Wednesday, July 27, 2016 10:22 AM
> To: rietveld_l@ill.fr
> Subject: CrySize error in TOPAS
>
> Dera friends,
>
> I'm doing Rietveld refinements in TOPAS; I get rather good fit of the
> reflections, rather good wt.%, but I've observed large errors for the
> CrySize (Lorentzian) values for some introduced Structures. I've tried to
> change it by refining CrySize (Gaussian), but it only changed in few
> particular cases. I'm rather sure that the intrumental parameters
> (geometry of the diffractometer was analyzed with the use of LaB6, Si, and
> other standards) and corrections (sample displ. etc.) are OK and I suppose
> these factors shouldn't influence (?) the CrySize values. I always
> constrain the minimum (20 starting value) and maximum (1 nm) value for
> CrySize; I usually refine strain, but I've noticed that it doesn't
> influence the results (at least the wt.% calculated). Rwp, goodness of fit
> and Durbin-Watson statistics R values are OK; also, the calculated
> background line is "flat", i.e., there is no mistaking of the background
> with reflections; the shapes of the reflections in the calculated
> diffractograms seem to be OK, too. I was thus wondering if these high
> errors coming from the CrySize are that important for the refinement?
>
> Best regards,
>
>
> --
> Łukasz Kruszewski, Ph.D., adjunct
> Polish Academy of Sciences
> Institute of Geological Sciences
> Twarda 51/55 str.
> 00-818 Warsaw
> Poland
>


-- 
Łukasz Kruszewski, Ph.D., adjunct
Polish Academy of Sciences
Institute of Geological Sciences
Twarda 51/55 str.
00-818 Warsaw
Poland
++
Please do NOT attach files to the whole list <alan.he...@neutronoptics.com>
Send commands to <lists...@ill.fr> eg: HELP as the subject with no body text
The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++

Re: CrySize error in TOPAS

[Saul Lapidus]

Also do you mean error (as in correct value) or calculated statistical
uncertainty?

Saul

On Wed, Jul 27, 2016 at 9:22 AM, "Łukasz Kruszewski"
 wrote:
> Dera friends,
>
> I'm doing Rietveld refinements in TOPAS; I get rather good fit of the
> reflections, rather good wt.%, but I've observed large errors for the
> CrySize (Lorentzian) values for some introduced Structures. I've tried to
> change it by refining CrySize (Gaussian), but it only changed in few
> particular cases. I'm rather sure that the intrumental parameters
> (geometry of the diffractometer was analyzed with the use of LaB6, Si, and
> other standards) and corrections (sample displ. etc.) are OK and I suppose
> these factors shouldn't influence (?) the CrySize values. I always
> constrain the minimum (20 starting value) and maximum (1 nm) value for
> CrySize; I usually refine strain, but I've noticed that it doesn't
> influence the results (at least the wt.% calculated). Rwp, goodness of fit
> and Durbin-Watson statistics R values are OK; also, the calculated
> background line is "flat", i.e., there is no mistaking of the background
> with reflections; the shapes of the reflections in the calculated
> diffractograms seem to be OK, too. I was thus wondering if these high
> errors coming from the CrySize are that important for the refinement?
>
> Best regards,
>
>
> --
> Łukasz Kruszewski, Ph.D., adjunct
> Polish Academy of Sciences
> Institute of Geological Sciences
> Twarda 51/55 str.
> 00-818 Warsaw
> Poland
>
> ++
> Please do NOT attach files to the whole list 
> Send commands to  eg: HELP as the subject with no body text
> The Rietveld_L list archive is on 
> http://www.mail-archive.com/rietveld_l@ill.fr/
> ++
>
>
++
Please do NOT attach files to the whole list 
Send commands to  eg: HELP as the subject with no body text
The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++

RE: CrySize error in TOPAS

[Cline, James Dr. (Fed)]

By what metric are you determining that the CrySize value is in error?


James P. Cline
Materials Measurement Science Division  
National Institute of Standards and Technology
100 Bureau Dr. stop 8520 [ B113 / Bldg 217 ]
Gaithersburg, MD 20899-8523    USA
jcl...@nist.gov
(301) 975 5793
FAX (301) 975 5334

-Original Message-
From: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] On Behalf Of 
"Lukasz Kruszewski"
Sent: Wednesday, July 27, 2016 10:22 AM
To: rietveld_l@ill.fr
Subject: CrySize error in TOPAS

Dera friends,

I'm doing Rietveld refinements in TOPAS; I get rather good fit of the 
reflections, rather good wt.%, but I've observed large errors for the CrySize 
(Lorentzian) values for some introduced Structures. I've tried to change it by 
refining CrySize (Gaussian), but it only changed in few particular cases. I'm 
rather sure that the intrumental parameters (geometry of the diffractometer was 
analyzed with the use of LaB6, Si, and other standards) and corrections (sample 
displ. etc.) are OK and I suppose these factors shouldn't influence (?) the 
CrySize values. I always constrain the minimum (20 starting value) and maximum 
(1 nm) value for CrySize; I usually refine strain, but I've noticed that it 
doesn't influence the results (at least the wt.% calculated). Rwp, goodness of 
fit and Durbin-Watson statistics R values are OK; also, the calculated 
background line is "flat", i.e., there is no mistaking of the background with 
reflections; the shapes of the reflections in the calculated diffractograms 
seem to be OK, too. I was thus wondering if these high errors coming from the 
CrySize are that important for the refinement?

Best regards,


--
Łukasz Kruszewski, Ph.D., adjunct
Polish Academy of Sciences
Institute of Geological Sciences
Twarda 51/55 str.
00-818 Warsaw
Poland
++
Please do NOT attach files to the whole list <alan.he...@neutronoptics.com>
Send commands to <lists...@ill.fr> eg: HELP as the subject with no body text
The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++

CrySize error in TOPAS

[Łukasz Kruszewski]

Dera friends,

I'm doing Rietveld refinements in TOPAS; I get rather good fit of the
reflections, rather good wt.%, but I've observed large errors for the
CrySize (Lorentzian) values for some introduced Structures. I've tried to
change it by refining CrySize (Gaussian), but it only changed in few
particular cases. I'm rather sure that the intrumental parameters
(geometry of the diffractometer was analyzed with the use of LaB6, Si, and
other standards) and corrections (sample displ. etc.) are OK and I suppose
these factors shouldn't influence (?) the CrySize values. I always
constrain the minimum (20 starting value) and maximum (1 nm) value for
CrySize; I usually refine strain, but I've noticed that it doesn't
influence the results (at least the wt.% calculated). Rwp, goodness of fit
and Durbin-Watson statistics R values are OK; also, the calculated
background line is "flat", i.e., there is no mistaking of the background
with reflections; the shapes of the reflections in the calculated
diffractograms seem to be OK, too. I was thus wondering if these high
errors coming from the CrySize are that important for the refinement?

Best regards,


-- 
Łukasz Kruszewski, Ph.D., adjunct
Polish Academy of Sciences
Institute of Geological Sciences
Twarda 51/55 str.
00-818 Warsaw
Poland
++
Please do NOT attach files to the whole list 
Send commands to  eg: HELP as the subject with no body text
The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++