Re: [Ifeffit] test/validation sample for air-sensitive sample cells?

2024-02-21 Thread Matthew Marcus 




 Fe2+ is notoriously sensitive. I think TiCl4 (a liquid) is used to test dryboxes because it hydrolyzes easily with production of white smoke if exposed to water vapor. If a small amount of this were mixed into a degassed binder, its XANES would




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Fe2+ is notoriously sensitive.  I think TiCl4 (a liquid) is used to test dryboxes because
it hydrolyzes easily with production of white smoke if exposed to water vapor.  If a small
amount of this were mixed into a degassed binder, its XANES would presumably show the
effect of hydrolysis.  As has been mentioned, Li-containing materials such as Li2FePO4
are sensitive.  Removing the Li by oxidation or hydrolysis would cause the Fe to oxidize
to Fe3+.

Sincerely,
 Matthew Marcus

On 2/21/2024 10:44 AM, Gerald T. Seidler wrote:
> Dear XAFS community, We've been developing air-sensitive sample cells for several of our XAFS experiments, but we don't have a good way of characterizing how well they actually reject air and water.   Does anyone have recommendations
> ZjQcmQRYFpfptBannerStart
> This Message Is From an External Sender
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> Dear XAFS community,
> We've been developing air-sensitive sample cells for several of our XAFS experiments, but we don't have a good way of characterizing how well they actually reject air and water.  Does anyone have recommendations for easily available 3d transition metal compounds that have a 'reasonable' amount of air sensitivity for purposes of sample call validation?  Any suggestions for other methods to validate performance? We would grind the sample and form a pellet with a degassed binder, in a glovebox or glovebag.
> With thanks,
> Jerry
> 
> -- 
> /Gerald Seidler/
> /Professor, Physics Department
> /
> /University of Washington/
> /https://urldefense.us/v3/__http://faculty.washington.edu/seidler/index.html__;!!G_uCfscf7eWS!ZQolBCsrtt913aAL9WhU7dEvTPIooBd701TPnC1xD2kIcsOp8Un_ZWV_vZCvkHrs0XerYlro8DB1A077YkXo_S8DmEFhhT9K$ 
>/
> /seid...@uw.edu /
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Re: [Ifeffit] test/validation sample for air-sensitive sample cells?

2024-02-21 Thread Lyle Gordon 
Hi Jerry,

I've seen people use various Li ion battery materials, lithium is nice, but
doesn't work here. Maybe NMC811 would work, it is unstable to exposure to
air and moisture. You could try some iron powder from a hand warmer pouch,
it will oxidize from ambient oxygen.

-Lyle

On Wed, Feb 21, 2024 at 1:35 PM Gerald T. Seidler  wrote:

> Dear XAFS community, We've been developing air-sensitive sample cells for
> several of our XAFS experiments, but we don't have a good way of
> characterizing how well they actually reject air and water.   Does anyone
> have recommendations
> ZjQcmQRYFpfptBannerStart
> This Message Is From an External Sender
> This message came from outside your organization.
>
> ZjQcmQRYFpfptBannerEnd
> Dear XAFS community,
> We've been developing air-sensitive sample cells for several of our XAFS
> experiments, but we don't have a good way of characterizing how well they
> actually reject air and water.  Does anyone have recommendations for easily
> available 3d transition metal compounds that have a 'reasonable' amount of
> air sensitivity for purposes of sample call validation?  Any suggestions
> for other methods to validate performance? We would grind the sample and
> form a pellet with a degassed binder, in a glovebox or glovebag.
> With thanks,
> Jerry
>
> --
> *Gerald Seidler*
>
> *Professor, Physics Department*
> *University of Washington*
>
> *https://urldefense.us/v3/__http://faculty.washington.edu/seidler/index.html__;!!G_uCfscf7eWS!eCvwFZmmEN_zoBONeI22H7RJ39nNzDl6pbZj4vkJCHaJ0xWs421UWvBpxrAzEo6deyBK4Ru3ctPb4DRaFuwvCoC9HkR5$
>  
> *
> *seid...@uw.edu *
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Re: [Ifeffit] test/validation sample for air-sensitive sample cells?

2024-02-21 Thread Chris Pollock 
Hi Jerry,
It's not a metal compound, but methyl viologen has always been my go-to for
anaerobic validation and has worked well for sample cells and glovebags and
such.

On Wed, Feb 21, 2024 at 4:35 PM Gerald T. Seidler  wrote:

> Dear XAFS community, We've been developing air-sensitive sample cells for
> several of our XAFS experiments, but we don't have a good way of
> characterizing how well they actually reject air and water.   Does anyone
> have recommendations
> ZjQcmQRYFpfptBannerStart
> This Message Is From an External Sender
> This message came from outside your organization.
>
> ZjQcmQRYFpfptBannerEnd
> Dear XAFS community,
> We've been developing air-sensitive sample cells for several of our XAFS
> experiments, but we don't have a good way of characterizing how well they
> actually reject air and water.  Does anyone have recommendations for easily
> available 3d transition metal compounds that have a 'reasonable' amount of
> air sensitivity for purposes of sample call validation?  Any suggestions
> for other methods to validate performance? We would grind the sample and
> form a pellet with a degassed binder, in a glovebox or glovebag.
> With thanks,
> Jerry
>
> --
> *Gerald Seidler*
>
> *Professor, Physics Department*
> *University of Washington*
>
> *https://urldefense.us/v3/__http://faculty.washington.edu/seidler/index.html__;!!G_uCfscf7eWS!YX3dFnQpB_Q0F0ozE34kmY5mpOvVR1bF27Hf7iUeX3W9gYhN2Bhsw0-HHMyBeF6k7sY9W9vgUBeDHZTYUGOXpBpO6kU4nhU$
>  
> *
> *seid...@uw.edu *
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[Ifeffit] test/validation sample for air-sensitive sample cells?

2024-02-21 Thread Gerald T. Seidler 
Dear XAFS community,
We've been developing air-sensitive sample cells for several of our XAFS
experiments, but we don't have a good way of characterizing how well they
actually reject air and water.  Does anyone have recommendations for easily
available 3d transition metal compounds that have a 'reasonable' amount of
air sensitivity for purposes of sample call validation?  Any suggestions
for other methods to validate performance? We would grind the sample and
form a pellet with a degassed binder, in a glovebox or glovebag.
With thanks,
Jerry

-- 
*Gerald Seidler*

*Professor, Physics Department*
*University of Washington*

*https://urldefense.us/v3/__http://faculty.washington.edu/seidler/index.html__;!!G_uCfscf7eWS!bc8I7gtiYjYV5xc8tbm1xHCOWp8emLi4nZo7rvTjsDdGw3JMBVgas9avdYSiT995CKzLi-eu2GCc0RfkE-Cz2uX2VeU-3A$
 
*
*seid...@uw.edu *
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