Re: [Ifeffit] SO2 for samples with non-planar geometry

2023-04-21 Thread Robert Gordon 
Didn't take the ln of the FLY by chance? ...after processing foil in 
transmission?


just trying to think of anything else

dead time of the FLY detector? (solid state assumed...DT correction 
applied?)


-R.

On 2023-04-21 7:31 p.m., Joel Brugger wrote:

Thanks Rob.,

Good thought, but definitively Cu++; we get the right energy shift and 
the right shape for XANES (linear Cu+ is very distinctive). We 
actually maintain nice oxidising conditions (4 bar of air applied to 
the capillary), and the spectra were stable over time (slew scan mode, 
with ~5 minutes per scan, and 10 scans collected).


Note that Cu+ is not stable in solution unless you give it a ligand 
such as chloride; reduction to Cu+ in our solution most likely would 
result in precipitation of Cu(0) via disproportionation. No evidence 
for this at all.



On 22 Apr 2023, at 12:14 pm, Robert Gordon  
wrote:


Hi Joel,

How much edge shift are you seeing between your foil and the solution?
Cu+2 is about 4.5 eV up from Cu metal...you seeing about that much?

Cu+2 can photoreduce...I know Cu+(aq) isn't stable, but maybe some 
complex is forming?

Just a thought...CN=2 and I think linear Cu+

-R.

On 2023-04-21 6:58 p.m., Joel Brugger wrote:

Capillary is silica glass :-)

On 22 Apr 2023, at 11:57 am, Anatoly Frenkel 
 wrote:


Capillary made or what?

Anatoly

On Apr 21, 2023, at 9:52 PM, Joel Brugger 
 wrote:


 Fluo, 0.5 wt% Cu.

On 22 Apr 2023, at 11:41 am, Anatoly Frenkel 
 wrote:


Fluorescence or transmission?
What is the Cu concentration? Could be self absorption.

Anatoly

On Apr 21, 2023, at 9:31 PM, Joel Brugger 
 wrote:


 Dear list,

We are trying to fit EXAFS from data collected on solutions 
within a capillary. The capillary has OD 1mm, ID 0.8mm, and was 
placed horizontally. The beam is 1x2 mm (VxH).


Fitting the copper reference foil, we get the expected SO2 value 
of ~0.7.


However, the solution containing the Cu(II) aqua ion gives a 
coordination of 2, instead of the expected 5-6. So our SO2 for 
this solution is apparently ~0.25.


I couldn’t find a discussion of the effect of geometry (in our 
case cylindrical rather than planar) on SO2. Is it possible that 
the low SO2 is a result of the odd geometry?


Confused as ever,

JOEL


*Joël Brugger*
Professor of Synchrotron Geosciences

*Monash University*
School of Earth, Atmosphere and Environment
Room 257A, Level 2, 9 Rainforest Walk 
Clayton, Victoria 3800 
Australia 

T: +61 3 9905 4898 
E: joel.brug...@monash.edu 
Twitter: @JoelBrugger

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Re: [Ifeffit] SO2 for samples with non-planar geometry

2023-04-21 Thread Joel Brugger 
Thanks Rob.,

Good thought, but definitively Cu++; we get the right energy shift and the 
right shape for XANES (linear Cu+ is very distinctive). We actually maintain 
nice oxidising conditions (4 bar of air applied to the capillary), and the 
spectra were stable over time (slew scan mode, with ~5 minutes per scan, and 10 
scans collected). 

Note that Cu+ is not stable in solution unless you give it a ligand such as 
chloride; reduction to Cu+ in our solution most likely would result in 
precipitation of Cu(0) via disproportionation. No evidence for this at all.


> On 22 Apr 2023, at 12:14 pm, Robert Gordon  wrote:
> 
> Hi Joel,
> 
> How much edge shift are you seeing between your foil and the solution?
> Cu+2 is about 4.5 eV up from Cu metal...you seeing about that much?
> 
> Cu+2 can photoreduce...I know Cu+(aq) isn't stable, but maybe some complex is 
> forming?
> Just a thought...CN=2 and I think linear Cu+
> 
> -R.
> 
> On 2023-04-21 6:58 p.m., Joel Brugger wrote:
>> Capillary is silica glass :-)
>> 
>>> On 22 Apr 2023, at 11:57 am, Anatoly Frenkel 
>>> mailto:anatoly.fren...@stonybrook.edu>> 
>>> wrote:
>>> 
>>> Capillary made or what?
>>> 
>>> Anatoly
>>> 
 On Apr 21, 2023, at 9:52 PM, Joel Brugger >>> > wrote:
 
  Fluo, 0.5 wt% Cu.
 
> On 22 Apr 2023, at 11:41 am, Anatoly Frenkel 
> mailto:anatoly.fren...@stonybrook.edu>> 
> wrote:
> 
> Fluorescence or transmission?
> What is the Cu concentration? Could be self absorption. 
> 
> Anatoly
> 
>> On Apr 21, 2023, at 9:31 PM, Joel Brugger > > wrote:
>> 
>>  Dear list,
>> 
>> We are trying to fit EXAFS from data collected on solutions within a 
>> capillary. The capillary has OD 1mm, ID 0.8mm, and was placed 
>> horizontally. The beam is 1x2 mm (VxH).
>> 
>> Fitting the copper reference foil, we get the expected SO2 value of ~0.7.
>> 
>> However, the solution containing the Cu(II) aqua ion gives a 
>> coordination of 2, instead of the expected 5-6. So our SO2 for this 
>> solution is apparently ~0.25. 
>> 
>> I couldn’t find a discussion of the effect of geometry (in our case 
>> cylindrical rather than planar) on SO2. Is it possible that the low SO2 
>> is a result of the odd geometry?
>> 
>> Confused as ever,
>> 
>> JOEL
>> 
>> 
>> Joël Brugger
>> Professor of Synchrotron Geosciences
>> 
>> Monash University
>> School of Earth, Atmosphere and Environment 
>> Room 257A, Level 2, 9 Rainforest Walk 
>> Clayton, Victoria 3800 
>> Australia 
>> 
>> T: +61 3 9905 4898 
>> E: joel.brug...@monash.edu  
>> Twitter: @JoelBrugger
>> 
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Re: [Ifeffit] SO2 for samples with non-planar geometry

2023-04-21 Thread Robert Gordon 

Hi Joel,

How much edge shift are you seeing between your foil and the solution?
Cu+2 is about 4.5 eV up from Cu metal...you seeing about that much?

Cu+2 can photoreduce...I know Cu+(aq) isn't stable, but maybe some 
complex is forming?

Just a thought...CN=2 and I think linear Cu+

-R.

On 2023-04-21 6:58 p.m., Joel Brugger wrote:

Capillary is silica glass :-)

On 22 Apr 2023, at 11:57 am, Anatoly Frenkel 
 wrote:


Capillary made or what?

Anatoly

On Apr 21, 2023, at 9:52 PM, Joel Brugger  
wrote:


 Fluo, 0.5 wt% Cu.

On 22 Apr 2023, at 11:41 am, Anatoly Frenkel 
 wrote:


Fluorescence or transmission?
What is the Cu concentration? Could be self absorption.

Anatoly

On Apr 21, 2023, at 9:31 PM, Joel Brugger 
 wrote:


 Dear list,

We are trying to fit EXAFS from data collected on solutions within 
a capillary. The capillary has OD 1mm, ID 0.8mm, and was placed 
horizontally. The beam is 1x2 mm (VxH).


Fitting the copper reference foil, we get the expected SO2 value 
of ~0.7.


However, the solution containing the Cu(II) aqua ion gives a 
coordination of 2, instead of the expected 5-6. So our SO2 for 
this solution is apparently ~0.25.


I couldn’t find a discussion of the effect of geometry (in our 
case cylindrical rather than planar) on SO2. Is it possible that 
the low SO2 is a result of the odd geometry?


Confused as ever,

JOEL


*Joël Brugger*
Professor of Synchrotron Geosciences

*Monash University*
School of Earth, Atmosphere and Environment
Room 257A, Level 2, 9 Rainforest Walk 
Clayton, Victoria 3800 
Australia 

T: +61 3 9905 4898 
E: joel.brug...@monash.edu 
Twitter: @JoelBrugger

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Re: [Ifeffit] SO2 for samples with non-planar geometry

2023-04-21 Thread Joel Brugger 
Capillary is silica glass :-)

> On 22 Apr 2023, at 11:57 am, Anatoly Frenkel  
> wrote:
> 
> Capillary made or what?
> 
> Anatoly
> 
>> On Apr 21, 2023, at 9:52 PM, Joel Brugger  wrote:
>> 
>> Fluo, 0.5 wt% Cu.
>> 
>>> On 22 Apr 2023, at 11:41 am, Anatoly Frenkel 
>>> mailto:anatoly.fren...@stonybrook.edu>> 
>>> wrote:
>>> 
>>> Fluorescence or transmission?
>>> What is the Cu concentration? Could be self absorption. 
>>> 
>>> Anatoly
>>> 
 On Apr 21, 2023, at 9:31 PM, Joel Brugger >>> > wrote:
 
 Dear list,
 
 We are trying to fit EXAFS from data collected on solutions within a 
 capillary. The capillary has OD 1mm, ID 0.8mm, and was placed 
 horizontally. The beam is 1x2 mm (VxH).
 
 Fitting the copper reference foil, we get the expected SO2 value of ~0.7.
 
 However, the solution containing the Cu(II) aqua ion gives a coordination 
 of 2, instead of the expected 5-6. So our SO2 for this solution is 
 apparently ~0.25. 
 
 I couldn’t find a discussion of the effect of geometry (in our case 
 cylindrical rather than planar) on SO2. Is it possible that the low SO2 is 
 a result of the odd geometry?
 
 Confused as ever,
 
 JOEL
 
 
 Joël Brugger
 Professor of Synchrotron Geosciences
 
 Monash University
 School of Earth, Atmosphere and Environment 
 Room 257A, Level 2, 9 Rainforest Walk 
 Clayton, Victoria 3800 
 Australia 
 
 T: +61 3 9905 4898 
 E: joel.brug...@monash.edu  
 Twitter: @JoelBrugger
 
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Re: [Ifeffit] SO2 for samples with non-planar geometry

2023-04-21 Thread Anatoly Frenkel 
Capillary made or what?AnatolyOn Apr 21, 2023, at 9:52 PM, Joel Brugger  wrote:Fluo, 0.5 wt% Cu.
On 22 Apr 2023, at 11:41 am, Anatoly Frenkel  wrote:Fluorescence or transmission?What is the Cu concentration? Could be self absorption. AnatolyOn Apr 21, 2023, at 9:31 PM, Joel Brugger  wrote:Dear list,We are trying to fit EXAFS from data collected on solutions within a capillary. The capillary has OD 1mm, ID 0.8mm, and was placed horizontally. The beam is 1x2 mm (VxH).Fitting the copper reference foil, we get the expected SO2 value of ~0.7.However, the solution containing the Cu(II) aqua ion gives a coordination of 2, instead of the expected 5-6. So our SO2 for this solution is apparently ~0.25. I couldn’t find a discussion of the effect of geometry (in our case cylindrical rather than planar) on SO2. Is it possible that the low SO2 is a result of the odd geometry?Confused as ever,JOEL
Joël BruggerProfessor of Synchrotron GeosciencesMonash UniversitySchool of Earth, Atmosphere and Environment Room 257A, Level 2, 9 Rainforest WalkClayton, Victoria 3800AustraliaT: +61 3 9905 4898E: joel.brug...@monash.edu Twitter: @JoelBrugger

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Re: [Ifeffit] SO2 for samples with non-planar geometry

2023-04-21 Thread Joel Brugger 
Fluo, 0.5 wt% Cu.

> On 22 Apr 2023, at 11:41 am, Anatoly Frenkel  > wrote:
> 
> Fluorescence or transmission?
> What is the Cu concentration? Could be self absorption. 
> 
> Anatoly
> 
>> On Apr 21, 2023, at 9:31 PM, Joel Brugger > > wrote:
>> 
>> Dear list,
>> 
>> We are trying to fit EXAFS from data collected on solutions within a 
>> capillary. The capillary has OD 1mm, ID 0.8mm, and was placed horizontally. 
>> The beam is 1x2 mm (VxH).
>> 
>> Fitting the copper reference foil, we get the expected SO2 value of ~0.7.
>> 
>> However, the solution containing the Cu(II) aqua ion gives a coordination of 
>> 2, instead of the expected 5-6. So our SO2 for this solution is apparently 
>> ~0.25. 
>> 
>> I couldn’t find a discussion of the effect of geometry (in our case 
>> cylindrical rather than planar) on SO2. Is it possible that the low SO2 is a 
>> result of the odd geometry?
>> 
>> Confused as ever,
>> 
>> JOEL
>> 
>> 
>> Joël Brugger
>> Professor of Synchrotron Geosciences
>> 
>> Monash University
>> School of Earth, Atmosphere and Environment 
>> Room 257A, Level 2, 9 Rainforest Walk 
>> Clayton, Victoria 3800 
>> Australia 
>> 
>> T: +61 3 9905 4898 
>> E: joel.brug...@monash.edu  
>> Twitter: @JoelBrugger
>> 
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Re: [Ifeffit] SO2 for samples with non-planar geometry

2023-04-21 Thread Anatoly Frenkel 
Fluorescence or transmission?What is the Cu concentration? Could be self absorption. AnatolyOn Apr 21, 2023, at 9:31 PM, Joel Brugger  wrote:Dear list,We are trying to fit EXAFS from data collected on solutions within a capillary. The capillary has OD 1mm, ID 0.8mm, and was placed horizontally. The beam is 1x2 mm (VxH).Fitting the copper reference foil, we get the expected SO2 value of ~0.7.However, the solution containing the Cu(II) aqua ion gives a coordination of 2, instead of the expected 5-6. So our SO2 for this solution is apparently ~0.25. I couldn’t find a discussion of the effect of geometry (in our case cylindrical rather than planar) on SO2. Is it possible that the low SO2 is a result of the odd geometry?Confused as ever,JOEL
Joël BruggerProfessor of Synchrotron GeosciencesMonash UniversitySchool of Earth, Atmosphere and Environment Room 257A, Level 2, 9 Rainforest WalkClayton, Victoria 3800AustraliaT: +61 3 9905 4898E: joel.brug...@monash.edu Twitter: @JoelBrugger

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[Ifeffit] SO2 for samples with non-planar geometry

2023-04-21 Thread Joel Brugger 
Dear list,

We are trying to fit EXAFS from data collected on solutions within a capillary. 
The capillary has OD 1mm, ID 0.8mm, and was placed horizontally. The beam is 
1x2 mm (VxH).

Fitting the copper reference foil, we get the expected SO2 value of ~0.7.

However, the solution containing the Cu(II) aqua ion gives a coordination of 2, 
instead of the expected 5-6. So our SO2 for this solution is apparently ~0.25. 

I couldn’t find a discussion of the effect of geometry (in our case cylindrical 
rather than planar) on SO2. Is it possible that the low SO2 is a result of the 
odd geometry?

Confused as ever,

JOEL


Joël Brugger
Professor of Synchrotron Geosciences

Monash University
School of Earth, Atmosphere and Environment 
Room 257A, Level 2, 9 Rainforest Walk 
Clayton, Victoria 3800 
Australia 

T: +61 3 9905 4898 
E: joel.brug...@monash.edu  
Twitter: @JoelBrugger



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