Re: [EXTERNAL] Mounting Sample on High Temperature XRD Ribbon Heater

[Mibeck, Blaise]

Been a long day. I did have a new platinum ribbon heater and it working well!

I would like to know this: how is the thermocouple attached to these ribbon 
heaters? (From Edmond- Buehler)

Thanks for any more advice. I really appreciate the help!

Get Outlook for Android<https://aka.ms/ghei36>


From: Julian Richard Tolchard 
Sent: Thursday, July 25, 2019 10:40:26 AM
To: Payzant, Andrew ; Mibeck, Blaise 
Cc: rietveld_l@ill.fr 
Subject: RE: [EXTERNAL] Mounting Sample on High Temperature XRD Ribbon Heater

Andrew,

I agree completely. Pt does definitely have its problems, but it's hard to get 
radiant heaters that go so high in temperature.

My feeling is that if you want to pursue HT-XRD in any serious fashion you need 
to accept the idea that Pt / Ta strips and thermocouples etc are "consumables" 
and live with the associated cost. I know this is difficult for a lot of 
university labs, but once you adopt that mindset you can do much more 
interesting experiments.


Jools


From: Payzant, Andrew 
Sent: torsdag 25. juli 2019 17.08
To: Julian Richard Tolchard ; Mibeck, Blaise 

Cc: rietveld_l@ill.fr
Subject: Re: [EXTERNAL] Mounting Sample on High Temperature XRD Ribbon Heater

Jools,

You are right. “Lab grade” bottled N2 may have enough residual oxygen to cause 
problems, plus it is hard to purge the chamber properly to get the pO2 low 
enough to avoid issues.  But an H2/N2 mix might not be suitable, especially if 
it destabilizes his sample. Here are some other ideas:


  1.  I used to flow high purity N2 through a gettering furnace in series with 
the HTXRD chamber, and that, coupled with multiple purges of the chamber prior 
to starting the experiment, worked pretty well.
  2.  I have in the past used a Bühler HT furnace that had a secondary 
“surround heater” option. I had some success putting a gettering wire across 
these leads and running it at a higher temperature than the heater strip in 
order to remove traces of oxygen from the chamber. This has the advantage that 
as you heat up the walls of the chamber and release adsorbed oxygen it goes to 
the getter rather than the strip. It can be a bit tricky ensuring that the 
getter is hotter than the strip across the range of temperatures that you run.

However, I fully agree with you that a platinum foil is probably a better 
option for Blaise’s experiment. If he has one handy.

There are some caveats regarding platinum though. It is generally more 
expensive. It is readily attacked by silicon, iron, and other elements. You can 
get recrystallization and/or rapid grain growth at high temperatures, which 
dramatically changes the diffraction pattern from the strip during a HTXRD 
experiment. The relatively high CTE means that the strip height will change as 
the temperature increases, which will cause large peak shifts unless you are 
using parallel beam optics and even then will cause intensity variations at the 
lower 2thetas. If you work at a US government lab, platinum is a precious metal 
and there is some paperwork required every time you change heater strips. Also, 
if your sample melts or sinters, you may have some “fun” getting the platinum 
clean.

Andrew

*

Dr. E. Andrew Payzant
Materials Engineering Group Leader
Neutron Scattering Division
Neutron Sciences Directorate

Mailing address:
Oak Ridge National Laboratory
Dr. E. Andrew Payzant
P.O. Box 2008
Bldg. 8600, MS 6475
Oak Ridge, TN 37831

cell: (865) 235-4981
email: payza...@ornl.gov<mailto:payza...@ornl.gov>
https://www.ornl.gov/staff-profile/e-andrew-payzant

**



From: Julian Richard Tolchard 
mailto:julianrichard.tolch...@sintef.no>>
Date: Thursday, July 25, 2019 at 10:47 AM
To: "Mibeck, Blaise" mailto:bmib...@undeerc.org>>, Andrew 
Payzant mailto:payza...@ornl.gov>>
Cc: Rietveld list mailto:rietveld_l@ill.fr>>
Subject: RE: [EXTERNAL] Mounting Sample on High Temperature XRD Ribbon Heater

Actually, i wouldn't recommend that either 😊

My experience with the Ta heaters is that they react with even the smallest 
amount of oxygen, and bottled N2 has more than enough to kill a Ta strip. The 
best result we had was with a H2/N2 mix, but that still failed (probably 
reaction with the sample).  Personally I think the only reliable way to use 
them is with a high vacuum system (turbo pump), and with relatively inert 
samples.

Ultimately you are better off getting a Pt strip instead.


Jools


From: rietveld_l-requ...@ill.fr<mailto:rietveld_l-requ...@ill.fr> 
mailto:rietveld_l-requ...@ill.fr>> On Behalf Of 
Mibeck, Blaise
Sent: torsdag 25. juli 2019 16.27
To: Payzant, Andrew mailto:payza...@ornl.gov>>
Cc: rietveld_l@ill.fr<mailto:rietveld_l@ill.fr>
Subject: Re: [EXTERNAL] Mounting Sample on High Temperature XRD Ribbon Heater

Thank you -- I will try nitrogen then

Re: [EXTERNAL] Mounting Sample on High Temperature XRD Ribbon Heater

[Mibeck, Blaise]

Thank you -- I will try nitrogen then!



From: Payzant, Andrew 
Sent: Thursday, July 25, 2019 9:08 AM
To: Mibeck, Blaise 
Cc: rietveld_l@ill.fr 
Subject: Re: [EXTERNAL] Mounting Sample on High Temperature XRD Ribbon Heater


STOP!!!



The tantalum foil should not be used for high temperature in air. Above a few 
hundred degrees Celsius it will oxidize rapidly and disintegrate.

I accidently learned this the hard way many years ago!  ?



Either use an inert atmosphere or vacuum. Or use a different heater ribbon, 
suitable for air atmosphere.



Andrew



*



Dr. E. Andrew Payzant

Materials Engineering Group Leader

Neutron Scattering Division

Neutron Sciences Directorate



Mailing address:

Oak Ridge National Laboratory

Dr. E. Andrew Payzant

P.O. Box 2008

Bldg. 8600, MS 6475

Oak Ridge, TN 37831



cell: (865) 235-4981

email: payza...@ornl.gov

https://www.ornl.gov/staff-profile/e-andrew-payzant



**







From:  on behalf of "Mibeck, Blaise" 

Reply-To: "Mibeck, Blaise" 
Date: Thursday, July 25, 2019 at 10:03 AM
To: Rietveld list 
Subject: [EXTERNAL] Mounting Sample on High Temperature XRD Ribbon Heater





I am looking for advice on how to prepar a HTXRD sample (mounting techniques, 
stage preparation, etc...). The ribbon heater is tantalum (brand new). The 
sample contained ammonium di-hydrogen phosphate. The atmosphere is air.



I hope to reach at least 1100C, but have had the ribbon break before 750C. 
Corrosion? or can the sample lower electrical resistance?



Please, any advice.



All the best,

Blaise








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++

Mounting Sample on High Temperature XRD Ribbon Heater

[Mibeck, Blaise]

I am looking for advice on how to prepar a HTXRD sample (mounting techniques, 
stage preparation, etc...). The ribbon heater is tantalum (brand new). The 
sample contained ammonium di-hydrogen phosphate. The atmosphere is air.

I hope to reach at least 1100C, but have had the ribbon break before 750C. 
Corrosion? or can the sample lower electrical resistance?

Please, any advice.

All the best,
Blaise




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++

XRF and XRD best practice...

[Mibeck, Blaise]

Hello all,

I use Rietveld primarily for quantitative phase analysis of rock samples. We 
collect XRF and XRD data on our samples.

Is there a best practice for using these data together? Or a recognized method 
or procedure for evaluating the agreement between the two? Can the XRF be used 
to restrain the phase concentrations in a refinement?

Thank you all for the years of advice I have gotten from this forum.

All the best,
Blaise

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RE: X-ray diffraction laboratory manager position [faked-from]

[Mibeck, Blaise]

Why are there so few job opportunities for people who have a Masters degree?

I believe this job would be ideal for a MS who has 5 or so years of lab 
experience.  




From: rietveld_l-requ...@ill.fr [rietveld_l-requ...@ill.fr] on behalf of Simon 
Redfern [s...@cam.ac.uk]
Sent: Friday, December 06, 2013 4:23 AM
To: rietveld_l@ill.fr
Subject: Re: X-ray diffraction laboratory manager position [faked-from]

Exactly so, Jon. This is the sort of job that a good candidate can make much 
of. I don't think it is described as a technician anywhere in the 
advertisement, but in any case, technical support jobs may require a high 
degree of training and education, so that in itself is not a discriminator. 
There are technicians and technicians, just as there are engineers and 
engineers.

Our X-ray lab manager has a PhD, is a skilled crystallographer, and deals with: 
instrument maintenance and support, new instrument planning, data analysis, 
interpretation, and scientific support to users who may not be expert. The role 
covers tuition to graduate students and outside users. It extends to 
scheduling, financial management, and reporting, and to contributions and 
authorship on some of the scientific papers that come out of the work of the 
lab. In many ways the role has similarities to a beam line scientist at a large 
scale facility, but with more reasonable working shift patterns (our X-ray lab 
manager actually also helps out in synchrotron and neutron campaigns).  Could 
beam line scientists be described as lab technicians? Not if you hope to return 
and get help with your next synchrotron/neutron experiment!

My observation is that for a proactive individual, this sort of position may 
offer significant scientific opportunities that extend well beyond wielding a 
screwdriver.

Simon Redfern

Professor of Mineral Physics
Department of Earth Sciences
University of Cambridge
Downing Street
Cambridge  CB2 3EQ  UK

w +44122475
m +447530312963
f +44122450


On 6 Dec 2013, at 08:32, Jonathan WRIGHT wrote:

> Did I click on the right link? The second point says:
>
> "Develop new experimental approaches and measurement routines as
> required by a growing user base."
>
> It doesn't sound so bad, unless the candidate can't think of any novel 
> experimental techniques to invent.
>
> Jon
>
>
> On 05/12/2013 19:02, Cline, James Dr. wrote:
>> Here is a position that looks a lot like what could be described as a
>> lab technician (no science anyway) and yet they require a PhD???
>>
>> How could anyone recommend a specialization in the powder diffraction
>> technique if this is all that is available?
>>
>> I find this very disconcerting.
>>
>> 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: rietveld_l-requ...@ill.fr
>> [mailto:rietveld_l-requ...@ill.fr] On Behalf Of Suchomel, Matthew R.
>> Sent: Tuesday, December 03, 2013 7:56 PM To: rietveld_l@ill.fr
>> Subject: Fwd: X-ray diffraction laboratory manager position
>>
>> Dear Colleagues
>>
>> On behalf of Prof. Jacob Jones, I am passing along the link below for
>> an open position of X-ray diffraction laboratory manager position at
>> North Carolina State University which may be of interest to someone
>> in our community.
>>
>> . X-ray diffraction laboratory manager:
>> https://jobs.ncsu.edu/postings/30892
>>
>>
>>
>> On Nov 27, 2013, at 14:46 , Jacob Jones  wrote:
>>
>> The Analytical Instrumentation Facility (AIF) at North Carolina State
>> University  is now seeking to fill multiple staff and postdoctoral
>> positions in the areas of electron microscopy and X-ray diffraction.
>> Positions are detailed in the links provided below. We are looking to
>> hire as soon as possible, but our first priority is finding the best
>> candidates to fill these positions. Please forward this information
>> to those who may have an interest in applying.
>>
>> . X-ray diffraction laboratory manager:
>> https://jobs.ncsu.edu/postings/30892
>>
>> Regards,
>>
>> Jacob L. Jones Associate Professor, Department of Materials Science
>> and Engineering Director, Analytical Instrumentation Facility North
>> Carolina State University Raleigh, NC Email: jacobjo...@ncsu.edu
>> Phone: 919-515-4557
>>
> ++
> Please do NOT attach files to the whole list 
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> http://www.mail-archive.com/rietveld_l@ill.fr/
> ++
>

++
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RE: how to extract %wts etc... from .lst file automatically... [SEC=PERSONAL]

[Mibeck, Blaise]

Thanks Max!
Problem solved!
Blaise


-Original Message-
From: AVDEEV, Maxim [mailto:m...@ansto.gov.au] 
Sent: Thursday, January 22, 2009 4:40 PM
To: Mibeck, Blaise
Subject: RE: how to extract %wts etc... from .lst file automatically...
[SEC=PERSONAL]

Hi Blaise,

If you like I can send you a small Fortran program I wrote for such data
extraction.

Cheers
Max

-
Max Avdeev

Instrument Scientist
Echidna High Resolution Powder Diffractometer
Bragg Institute, Building 87
Australian Nuclear Science and Technology Organisation
PMB 1, Menai NSW 2234
AUSTRALIA
T +61 2 9717 9522
F +61 2 9717 3606
E m...@ansto.gov.au
www.ansto.gov.au/research/bragg_institute.html
  
-Original Message-
From: Mibeck, Blaise [mailto:bmib...@undeerc.org] 
Sent: Friday, January 23, 2009 9:19 AM
To: rietveld_l@ill.fr
Subject: how to extract %wts etc... from .lst file automatically... 



Hello, 

Using GSAS, I now have hundreds of *.lst files - I have done my
refinements with quantitative phase analysis being my goal. 

I could go into each .lst file and cut and paste the %weights and sigmas
for each phase into a spread sheet. I could try to write a program that
does this and reports the phase names with %wts. 

Is there a feature in GSAS (or Expgui) for generating reports for
quantitative phase analysis? If not, is there a program or utility
available that does this??

I just need the values (%wt and sigma) reported by GSAS for each phase
in an experiment file - I am applying micro-absorption corrections by
spread sheet. If you know of a program that would allow me to report
other data, this would be welcomed as well.  

All the Best, 
Blaise

* * * * * * * * * * * * * 
Blaise Mibeck 
Research Scientist
Energy & Environmental Research Center
University of North Dakota
15 North 23rd Street, Stop 9018
Grand Forks, ND 58202-9018

Phone: (701) 777-5077
Email: bmib...@undeerc.org

how to extract %wts etc... from .lst file automatically...

[Mibeck, Blaise]

 

Hello, 

 

Using GSAS, I now have hundreds of *.lst files - I have done my
refinements with quantitative phase analysis being my goal. 

 

I could go into each .lst file and cut and paste the %weights and sigmas
for each phase into a spread sheet. I could try to write a program that
does this and reports the phase names with %wts. 

 

Is there a feature in GSAS (or Expgui) for generating reports for
quantitative phase analysis? If not, is there a program or utility
available that does this??

 

I just need the values (%wt and sigma) reported by GSAS for each phase
in an experiment file - I am applying micro-absorption corrections by
spread sheet. If you know of a program that would allow me to report
other data, this would be welcomed as well.  

 

All the Best, 

Blaise

 

* * * * * * * * * * * * * 

Blaise Mibeck 

Research Scientist

Energy & Environmental Research Center

University of North Dakota

15 North 23rd Street, Stop 9018

Grand Forks, ND 58202-9018

 

Phone: (701) 777-5077

Email: bmib...@undeerc.org

 

 

 

RE: Quantitative analysis

[Mibeck, Blaise]

 

I am learning QPA and am worried about PO. 

 

I wonder why sample spinning isn't discussed more. 

 

I am luckily able to barrow time on a newer diffractometer with a sample
spinner. 

 

Does this reduce PO? Or completely eliminate it? There is a set up
variable in GSAS for whether you are spinning the sample - are there
guidelines for how many revolutions to spin the sample if you just want
to reduce PO?

 

Thanks to all for there help!!!

Blaise

 

 

 

 

* * * * * * * * * * * * * 

Blaise Mibeck 

Research Scientist

Energy & Environmental Research Center

University of North Dakota

15 North 23rd Street, Stop 9018

Grand Forks, ND 58202-9018

 

Phone: (701) 777-5077

Email: [EMAIL PROTECTED]

 

 

-Original Message-
From: David L. Bish [mailto:[EMAIL PROTECTED] 
Sent: Tuesday, October 28, 2008 9:09 AM
To: Martin; [EMAIL PROTECTED]; rietveld_l@ill.fr
Subject: RE: Quantitative analysis

 

I agree that it's always best to avoid preferred orientation, but that
is easier said than done on a routine basis.  I have personally had good
luck with the M-D PO correction on many known samples, as long as the PO
was not severe.

However, I imagine that Mario's problems are related to microabsorption
in this case.  Mario, if you can re-measure your data with a Co or Fe
tube, it would be a good test of this.

Dave Bish

At 08:51 AM 10/28/2008 -0400, Martin wrote:



Sorry to disagree. Experience tells me otherwise - the March-Dollase
correction has nearly always led to poor quant results for me. It most
certainly cannot be applied safely.
 
Martin
 
--
 
M Vickers
Dept of Chemistry
UCL






> Subject: Re: Quantitative analysis
> Date: Tue, 28 Oct 2008 02:53:20 -0700
> From: [EMAIL PROTECTED]
> To: Rietveld_l@ill.fr
> 
> Dear Mario,
> 
> One more possible problem of applying preferred orientation
corrections in QPA is that not all of them are normalized. For example,
the March-Dollase correction is normalized and can be applied safely,
but the Rietveld-Toraya correction is inapplicable to QPA as it does not
preserve the scale normalization. 
> 
> Best regards,
> Leonid
> 
> ***
> Leonid A. Solovyov
> Institute of Chemistry and Chemical Technology
> K. Marx av., 42
> 660049, Krasnoyarsk Russia
> Phone: +7 3912 495663
> Fax: +7 3912 238658
> www.icct.ru/eng/content/persons/Sol_LA
> 



For the best free wallpapers from MSN Click here!
  

Beginer problems, difficulty charecterizing our diffractometer...

[Mibeck, Blaise]

 

I am re-learning GSAS to bring Rietveld to my department (for the first
time). We have an old Phillips Xpert. 

 

I am trying to refine a quartz standard to acquire my profile and instrument
parameters for this instrument and have yet to get my Chi^2 below 500. The
instrument is not in my direct control. I have caught and asked them to
correct a few problems already (dwell time too low, aluminum sneaking into
the beam, etc...) and this has helped. I would like not to annoy them any
more than I have too. 

 

At this point I think my high Chi^2s are mainly due to low angle asymmetric
peaks that my fit is not able to copy - the asym is not terrible but may be
messing me up. I am getting better results with peak profile functions 3 and
4, but unable to get Chi^2 below 500. My scans go up to 70 degrees 2theta.

 

I would like to tell the people caring for the instrument that my problem is
on their end, but I am not confident in my own refining skills to say this.
When I work with the tutorials or standard data from my graduate school
experiment I am ok - I think I am proceeding in a reasonable way, although I
can get stuck here and there. 

 

I would like to find out if I am doing something incorrectly or if the
problem is instrument related. I hate to bug one of you but wonder if I
could get someone to look at my work?? Is there a better forum for asking
for this kind of help? 

 

Kindest regards to all of you,

Blaise

 

 

 

 

 

 

* * * * * * * * * * * * * 

Blaise Mibeck 

Research Scientist

Energy & Environmental Research Center

University of North Dakota

15 North 23rd Street, Stop 9018

Grand Forks, ND 58202-9018

 

Phone: (701) 777-5077

Email: [EMAIL PROTECTED]  

 

 

 

RE: Question about Genles...

[Mibeck, Blaise]

 

Thanks!!! 

 

 

-Original Message-
From: Davide Levy [mailto:[EMAIL PROTECTED] 
Sent: Tuesday, September 09, 2008 12:51 PM
To: Mibeck, Blaise
Subject: R: Question about Genles...

 

Dear Blaise, 

that means that your parameters are not appropriate (generally too big)  for
format defined in the Fortran code.  If it always happens you should edit
the .EXP file with a text editor and check if there is any 1.#R instead a
numeric parameter.

Davide

 

Da: Mibeck, Blaise [mailto:[EMAIL PROTECTED] 
Inviato: martedì 9 settembre 2008 19.28
A: rietveld_l@ill.fr
Oggetto: Question about Genles...

 

Regarding GSAS: 

 

Most of the time when I make inappropriate changes in my refinement
sequence, the refinement in genles diverges. Occasionally, however, I see
Chi^2 = 1.#QNB and sum((shift.esd)^2) line out at 1.#R.

 

I have been assuming that I messed up my refinement order, or allowed
incompatible parameters to vary. So I back up and trudge on. In other words
I treat the problem as if Genles diverged.

 

Should Genles be diverging? Do these values (more like symbols) mean
anything? Or is something corrupted or not set correctly on my installation?


 

Thanks for your help on my last question by the way --- I greatly appreciate
this forum!

 

Kindest regards,

Blaise

 

 

 

 

* * * * * * * * * * * * * 

Blaise Mibeck 

Research Scientist

Energy & Environmental Research Center

University of North Dakota

15 North 23rd Street, Stop 9018

Grand Forks, ND 58202-9018

 

Phone: (701) 777-5077

Email: [EMAIL PROTECTED] <mailto:[EMAIL PROTECTED]> 

 

 

 

Question about Genles...

[Mibeck, Blaise]

Regarding GSAS: 

 

Most of the time when I make inappropriate changes in my refinement
sequence, the refinement in genles diverges. Occasionally, however, I see
Chi^2 = 1.#QNB and sum((shift.esd)^2) line out at 1.#R.

 

I have been assuming that I messed up my refinement order, or allowed
incompatible parameters to vary. So I back up and trudge on. In other words
I treat the problem as if Genles diverged.

 

Should Genles be diverging? Do these values (more like symbols) mean
anything? Or is something corrupted or not set correctly on my installation?


 

Thanks for your help on my last question by the way --- I greatly appreciate
this forum!

 

Kindest regards,

Blaise

 

 

 

 

* * * * * * * * * * * * * 

Blaise Mibeck 

Research Scientist

Energy & Environmental Research Center

University of North Dakota

15 North 23rd Street, Stop 9018

Grand Forks, ND 58202-9018

 

Phone: (701) 777-5077

Email: [EMAIL PROTECTED]  

 

 

 

RE: Portable XRD

[Mibeck, Blaise]

 

 

I am relearning GSAS right now. I was pretty good at it in graduate school
(DOS-GSAS). I have PC-GSAS running and everything works -- but I am having
trouble getting use to the program being in the windows environment. 

 

I know this is a stupid request: can I still get the dos version? Or is it
possible to run PC-GSAS in dos? In other words can I make the entire program
entirely command line? My fingers are twitching to go faster and my mouse is
getting in the way.  

 

I feel like my dad when he asked me to upgrade his work laptop from windows
95 to windows 3.x. :-)  

 

Kind regards to all! 

Blaise

 

 

 

 

 

* * * * * * * * * * * * * 

Blaise Mibeck 

Research Scientist

Energy & Environmental Research Center

University of North Dakota

15 North 23rd Street, Stop 9018

Grand Forks, ND 58202-9018

 

Phone: (701) 777-5077

Email: [EMAIL PROTECTED]