Preparation help with fly ash sample with diluted Tl

Mengling Yi Stuckman

29 Sep 2011 29 Sep '11

9:39 a.m.

Dear Ifeffit Community, I am currently working on project "Evaluating Speciation of Thallium in Coal Fly Ash". The project was accepted by APS and we will conduct our measurement on beamline 5-BM-D. My fly ash sample has Tl concentration ranging from 0.5ppm to 13ppm. How can I know whether the sample can generate enough photon counts if using fluorescence mode? what would be the appropriate sample preparation procedure I should follow? Is there any interference I should pay attention to? I understand that I should use Hephaestus, but I don't know how to do that if my sample contains lots of different oxides. I attached the elemental composition in this email. Most metals should be in form of oxides, or sulfates. Any input would be highly appreciated, Mengling

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CardinalandConsvilleFlyAshComposition1.xls (application/vnd.ms-excel — 30.0 KB)

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"Dr. Dariusz A. Zając"

29 Sep 29 Sep

10 a.m.

Dear Mengling, I suppose you should contact beamline responsible and ask about beamline limitations (intensity of the beam at Tl edge, detector sensitivity, etc). Normally it is done before sending the project... Sample preparation for fluorescence, in your case should be, in general, to condense your sample as much as possible (I didnt look at your xls file!) in respect to the minerals you have... What do you want to calculate using Hephaestus? best regards kicaj W dniu 11-09-29 16:39, Mengling Yi Stuckman pisze:

...

Dear Ifeffit Community, I am currently working on project "Evaluating Speciation of Thallium in Coal Fly Ash". The project was accepted by APS and we will conduct our measurement on beamline 5-BM-D. My fly ash sample has Tl concentration ranging from 0.5ppm to 13ppm. How can I know whether the sample can generate enough photon counts if using fluorescence mode? what would be the appropriate sample preparation procedure I should follow? Is there any interference I should pay attention to? I understand that I should use Hephaestus, but I don't know how to do that if my sample contains lots of different oxides. I attached the elemental composition in this email. Most metals should be in form of oxides, or sulfates. Any input would be highly appreciated, Mengling

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Matt Newville

10:02 a.m.

Dear Mengling, The basic issues are: will there be enough Tl fluorescence counts in the detector, and will you be able to see a decent edge. From you spreadsheet of concentrations, the elements that stand out are: Fe and to a lesser extent Zn, and Pb. The Fe and Zn will dominate the fluorescence getting to your detector. This hurts sensitivity to Tl because the solid-state detectors can handle a limited flux themselves (typically on the order of 100K Hz). The high Fe concentration means the Fe Kalpha will dominate the emission when you shine 12.7keV x-rays on the sample. The simple-but-effective remedy is to put aluminum foil on the detector, as aluminum will absorb Fe fluorescence (at 6.4keV) about 4x more than the Tl fluorescence (at 10.3keV). You might need a few hundred microns of aluminum foil, and may need to try a few different amounts to cut down the Fe counts sufficiently. The other issue is Pb. The Tl L3 edge is at 12.658keV. once you hit the Pb L3 edge, at 13.1 keV, the Pb Lalpha fluorescence will dominate the Tl Lalpha fluorescence -- these lines (10.3 and 10.5 keV, respectively) are too close together to effectively filter electronically. Even well below the Pb L3 edge, you'll start to see some Pb Lalpha fluorescence. Since the Pb concentration might be 100x the Tl concentration, that would be something to look for, but there's not a lot that can be done about it. Anyway, that really only limits the EXAFS, not so much the ability to get XANES. The Tl concentrations are low, but I think that at a good APS BM line like 5-BM, getting Tl L3 XANES is just a matter of time. Hope that helps, --Matt On Thu, Sep 29, 2011 at 9:39 AM, Mengling Yi Stuckman wrote:

...

Dear Ifeffit Community,

I am currently working on project "Evaluating Speciation of Thallium in Coal Fly Ash". The project was accepted by APS and we will conduct our measurement on beamline 5-BM-D.

My fly ash sample has Tl concentration ranging from 0.5ppm to 13ppm. How can I know whether the sample can generate enough photon counts if using fluorescence mode? what would be the appropriate sample preparation procedure I should follow? Is there any interference I should pay attention to?

I understand that I should use Hephaestus, but I don't know how to do that if my sample contains lots of different oxides. I attached the elemental composition in this email. Most metals should be in form of oxides, or sulfates.

Any input would be highly appreciated,

Mengling

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"Dr. Dariusz A. Zając"

1:15 p.m.

Dear Matt, this is very good introduction for fluorescence measurements on diluted samples... Like a tutorial... I just want to add small comments: as I understood the sample is an ash, so maybe will be possible to condense it, e.g. press it into the pellet. If there will be no possible to measure exafs (due to heavier elements), and is needed to focus on xanes, than I suggest to use non-energy dispersive detector, e.g. PIPS diode. It is very often more sensitive than regular fluorescence detectors, and can take higher count-rate. please correct me if I am wrong... kicaj W dniu 11-09-29 17:02, Matt Newville pisze:

...

Dear Mengling,

The basic issues are: will there be enough Tl fluorescence counts in the detector, and will you be able to see a decent edge. From you spreadsheet of concentrations, the elements that stand out are: Fe and to a lesser extent Zn, and Pb.

The Fe and Zn will dominate the fluorescence getting to your detector. This hurts sensitivity to Tl because the solid-state detectors can handle a limited flux themselves (typically on the order of 100K Hz). The high Fe concentration means the Fe Kalpha will dominate the emission when you shine 12.7keV x-rays on the sample. The simple-but-effective remedy is to put aluminum foil on the detector, as aluminum will absorb Fe fluorescence (at 6.4keV) about 4x more than the Tl fluorescence (at 10.3keV). You might need a few hundred microns of aluminum foil, and may need to try a few different amounts to cut down the Fe counts sufficiently.

The other issue is Pb. The Tl L3 edge is at 12.658keV. once you hit the Pb L3 edge, at 13.1 keV, the Pb Lalpha fluorescence will dominate the Tl Lalpha fluorescence -- these lines (10.3 and 10.5 keV, respectively) are too close together to effectively filter electronically. Even well below the Pb L3 edge, you'll start to see some Pb Lalpha fluorescence. Since the Pb concentration might be 100x the Tl concentration, that would be something to look for, but there's not a lot that can be done about it. Anyway, that really only limits the EXAFS, not so much the ability to get XANES. The Tl concentrations are low, but I think that at a good APS BM line like 5-BM, getting Tl L3 XANES is just a matter of time.

Hope that helps,

--Matt

On Thu, Sep 29, 2011 at 9:39 AM, Mengling Yi Stuckman wrote:

...
Dear Ifeffit Community,

I am currently working on project "Evaluating Speciation of Thallium in Coal Fly Ash". The project was accepted by APS and we will conduct our measurement on beamline 5-BM-D.

My fly ash sample has Tl concentration ranging from 0.5ppm to 13ppm. How can I know whether the sample can generate enough photon counts if using fluorescence mode? what would be the appropriate sample preparation procedure I should follow? Is there any interference I should pay attention to?

I understand that I should use Hephaestus, but I don't know how to do that if my sample contains lots of different oxides. I attached the elemental composition in this email. Most metals should be in form of oxides, or sulfates.

Any input would be highly appreciated,

Mengling

_______________________________________________ Ifeffit mailing list Ifeffit@millenia.cars.aps.anl.gov http://millenia.cars.aps.anl.gov/mailman/listinfo/ifeffit

_______________________________________________ Ifeffit mailing list Ifeffit@millenia.cars.aps.anl.gov http://millenia.cars.aps.anl.gov/mailman/listinfo/ifeffit

Mengling Yi Stuckman

4:43 p.m.

Thanks for all the response! They are all very helpful! Just want to make sure that I get the information right and a few follow-up questions: 1. I'd better contact the beamline engineer to ask for the sensitivity for Tl. 2. Fe fluorescence interference could be decreased by adding a few layer of Al foil. I knew that I did that when I measured As fluorescence. So this is ok. 3. Pb fluorescence interference is very hard to eliminate. Therefore, EXAFS for Tl is very hard to get. Actually, I didn't see any papers on Tl EXAFS and maybe that is why. The research question I want to answer is: what structure Tl is bond to in the fly ash? Tl(I) and Tl(III) could theoretically bind to sulfate, nitrate, bicarbonate, etc.. I saw some papers that are using nitrate, sulfate, bicarbonate Tl salt as references for micro-XANES measurement. And then they compared the XANES in the end. Is that a better approach than EXAFS to answer the question? 4. To increase the intensity, we can condense the ash by pressing it into pellet. The fly ash from coal combustion power plants are already pretty compacted. They are mainly gypsum in most cases. I dont' know if that helps or not. 5. This is the first time I heard about non-energy dispersive detector, e.g. PIPS diode. We are planning to use 13-element detector. What is the advantage of using one way or the other? If I do want to concentrate on XANES, would be helpful to ask the beamline engineer for the possibility of changing detectors? Thank you all again, Mengling 2011/9/29 "Dr. Dariusz A. Zając"

...

Dear Matt, this is very good introduction for fluorescence measurements on diluted samples... Like a tutorial... I just want to add small comments: as I understood the sample is an ash, so maybe will be possible to condense it, e.g. press it into the pellet. If there will be no possible to measure exafs (due to heavier elements), and is needed to focus on xanes, than I suggest to use non-energy dispersive detector, e.g. PIPS diode. It is very often more sensitive than regular fluorescence detectors, and can take higher count-rate. please correct me if I am wrong... kicaj

W dniu 11-09-29 17:02, Matt Newville pisze:

Dear Mengling,

...
The basic issues are: will there be enough Tl fluorescence counts in the detector, and will you be able to see a decent edge. From you spreadsheet of concentrations, the elements that stand out are: Fe and to a lesser extent Zn, and Pb.

The Fe and Zn will dominate the fluorescence getting to your detector. This hurts sensitivity to Tl because the solid-state detectors can handle a limited flux themselves (typically on the order of 100K Hz). The high Fe concentration means the Fe Kalpha will dominate the emission when you shine 12.7keV x-rays on the sample. The simple-but-effective remedy is to put aluminum foil on the detector, as aluminum will absorb Fe fluorescence (at 6.4keV) about 4x more than the Tl fluorescence (at 10.3keV). You might need a few hundred microns of aluminum foil, and may need to try a few different amounts to cut down the Fe counts sufficiently.

The other issue is Pb. The Tl L3 edge is at 12.658keV. once you hit the Pb L3 edge, at 13.1 keV, the Pb Lalpha fluorescence will dominate the Tl Lalpha fluorescence -- these lines (10.3 and 10.5 keV, respectively) are too close together to effectively filter electronically. Even well below the Pb L3 edge, you'll start to see some Pb Lalpha fluorescence. Since the Pb concentration might be 100x the Tl concentration, that would be something to look for, but there's not a lot that can be done about it. Anyway, that really only limits the EXAFS, not so much the ability to get XANES. The Tl concentrations are low, but I think that at a good APS BM line like 5-BM, getting Tl L3 XANES is just a matter of time.

Hope that helps,

--Matt

On Thu, Sep 29, 2011 at 9:39 AM, Mengling Yi Stuckman wrote:

...
Dear Ifeffit Community,

I am currently working on project "Evaluating Speciation of Thallium in Coal Fly Ash". The project was accepted by APS and we will conduct our measurement on beamline 5-BM-D.

My fly ash sample has Tl concentration ranging from 0.5ppm to 13ppm. How can I know whether the sample can generate enough photon counts if using fluorescence mode? what would be the appropriate sample preparation procedure I should follow? Is there any interference I should pay attention to?

I understand that I should use Hephaestus, but I don't know how to do that if my sample contains lots of different oxides. I attached the elemental composition in this email. Most metals should be in form of oxides, or sulfates.

Any input would be highly appreciated,

Mengling

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-- Mengling Yi Stuckman Graduate Research Assistant Civil and Environmental Engineering and Geodetic Science Ohio State University 2070 Neil Ave., Columbus, OH, 43210

Matt Newville

7 p.m.

Hi Mengling, 2011/9/29 Mengling Yi Stuckman :

...

Thanks for all the response! They are all very helpful! Just want to make sure that I get the information right and a few follow-up questions: 1. I'd better contact the beamline engineer to ask for the sensitivity for Tl.

Yes!

...

2. Fe fluorescence interference could be decreased by adding a few layer of Al foil. I knew that I did that when I measured As fluorescence. So this is ok.

Yes.

...

3. Pb fluorescence interference is very hard to eliminate. Therefore, EXAFS for Tl is very hard to get. Actually, I didn't see any papers on Tl EXAFS and maybe that is why. The research question I want to answer is: what structure Tl is bond to in the fly ash? Tl(I) and Tl(III) could theoretically bind to sulfate, nitrate, bicarbonate, etc.. I saw some papers that are using nitrate, sulfate, bicarbonate Tl salt as references for micro-XANES measurement. And then they compared the XANES in the end. Is that a better approach than EXAFS to answer the question?

Well, maybe not "better", but generally tolerant of less good data. And also generally more "directly sensitive" to oxidation state and ligand. I won't kid you though - Hg, Tl, and Pb L3 XANES can be tricky to analyze well, as the features are not very well resolved.

...

4. To increase the intensity, we can condense the ash by pressing it into pellet. The fly ash from coal combustion power plants are already pretty compacted. They are mainly gypsum in most cases. I dont' know if that helps or not.

It won't hurt.

...

5. This is the first time I heard about non-energy dispersive detector, e.g. PIPS diode. We are planning to use 13-element detector. What is the advantage of using one way or the other? If I do want to concentrate on XANES, would be helpful to ask the beamline engineer for the possibility of changing detectors?

I'd start with the 13-element Ge detector and see how that goes.... Cheers, --Matt

Mengling Yi Stuckman

9:33 p.m.

Thank you so much! This is the first time I tried to use ifeffit mailing list. I would have never expected so many responses from so many scientists. I wish one day I could be able to contribute back to this great scientific community as well! Thanks again! Mengling On Thu, Sep 29, 2011 at 8:00 PM, Matt Newville wrote:

...

Hi Mengling,

2011/9/29 Mengling Yi Stuckman :

...
Thanks for all the response! They are all very helpful! Just want to make sure that I get the information right and a few follow-up questions: 1. I'd better contact the beamline engineer to ask for the sensitivity for Tl.

Yes!

...
2. Fe fluorescence interference could be decreased by adding a few layer of Al foil. I knew that I did that when I measured As fluorescence. So this is ok.

Yes.

...
3. Pb fluorescence interference is very hard to eliminate. Therefore, EXAFS for Tl is very hard to get. Actually, I didn't see any papers on Tl EXAFS and maybe that is why. The research question I want to answer is: what structure Tl is bond to in the fly ash? Tl(I) and Tl(III) could theoretically bind to sulfate, nitrate, bicarbonate, etc.. I saw some papers that are using nitrate, sulfate, bicarbonate Tl salt as references for micro-XANES measurement. And then they compared the XANES in the end. Is that a better approach than EXAFS to answer the question?

Well, maybe not "better", but generally tolerant of less good data. And also generally more "directly sensitive" to oxidation state and ligand. I won't kid you though - Hg, Tl, and Pb L3 XANES can be tricky to analyze well, as the features are not very well resolved.

...
4. To increase the intensity, we can condense the ash by pressing it into pellet. The fly ash from coal combustion power plants are already pretty compacted. They are mainly gypsum in most cases. I dont' know if that helps or not.

It won't hurt.

...
5. This is the first time I heard about non-energy dispersive detector, e.g. PIPS diode. We are planning to use 13-element detector. What is the advantage of using one way or the other? If I do want to concentrate on XANES, would be helpful to ask the beamline engineer for the possibility of changing detectors?

I'd start with the 13-element Ge detector and see how that goes....

Cheers,

--Matt

_______________________________________________ Ifeffit mailing list Ifeffit@millenia.cars.aps.anl.gov http://millenia.cars.aps.anl.gov/mailman/listinfo/ifeffit

-- Mengling Yi Stuckman Graduate Research Assistant Civil and Environmental Engineering and Geodetic Science Ohio State University 2070 Neil Ave., Columbus, OH, 43210

Matt Newville

6:51 p.m.

Hi Dariusz, Thanks, those are good suggestions. I was assuming that they'd use a solid state (say 10+ element Ge) detector for concentrations at and below 10 ppm. A large diode detector might work OK -- they can often take higher total count rate at the expense of energy discrimination. I'd be happy to be shown a comparison, but my guess is that electronically removing the Fe and Compton scattering would be worth the effort for these concentrations. --Matt 2011/9/29 "Dr. Dariusz A. Zając" :

...

Dear Matt, this is very good introduction for fluorescence measurements on diluted samples... Like a tutorial... I just want to add small comments: as I understood the sample is an ash, so maybe will be possible to condense it, e.g. press it into the pellet. If there will be no possible to measure exafs (due to heavier elements), and is needed to focus on xanes, than I suggest to use non-energy dispersive detector, e.g. PIPS diode. It is very often more sensitive than regular fluorescence detectors, and can take higher count-rate. please correct me if I am wrong... kicaj

W dniu 11-09-29 17:02, Matt Newville pisze:

...
Dear Mengling,

The basic issues are: will there be enough Tl fluorescence counts in the detector, and will you be able to see a decent edge. From you spreadsheet of concentrations, the elements that stand out are: Fe and to a lesser extent Zn, and Pb.

The Fe and Zn will dominate the fluorescence getting to your detector. This hurts sensitivity to Tl because the solid-state detectors can handle a limited flux themselves (typically on the order of 100K Hz). The high Fe concentration means the Fe Kalpha will dominate the emission when you shine 12.7keV x-rays on the sample. The simple-but-effective remedy is to put aluminum foil on the detector, as aluminum will absorb Fe fluorescence (at 6.4keV) about 4x more than the Tl fluorescence (at 10.3keV). You might need a few hundred microns of aluminum foil, and may need to try a few different amounts to cut down the Fe counts sufficiently.

The other issue is Pb. The Tl L3 edge is at 12.658keV. once you hit the Pb L3 edge, at 13.1 keV, the Pb Lalpha fluorescence will dominate the Tl Lalpha fluorescence -- these lines (10.3 and 10.5 keV, respectively) are too close together to effectively filter electronically. Even well below the Pb L3 edge, you'll start to see some Pb Lalpha fluorescence. Since the Pb concentration might be 100x the Tl concentration, that would be something to look for, but there's not a lot that can be done about it. Anyway, that really only limits the EXAFS, not so much the ability to get XANES. The Tl concentrations are low, but I think that at a good APS BM line like 5-BM, getting Tl L3 XANES is just a matter of time.

Hope that helps,

--Matt

On Thu, Sep 29, 2011 at 9:39 AM, Mengling Yi Stuckman wrote:

...
Dear Ifeffit Community,

I am currently working on project "Evaluating Speciation of Thallium in Coal Fly Ash". The project was accepted by APS and we will conduct our measurement on beamline 5-BM-D.

My fly ash sample has Tl concentration ranging from 0.5ppm to 13ppm. How can I know whether the sample can generate enough photon counts if using fluorescence mode? what would be the appropriate sample preparation procedure I should follow? Is there any interference I should pay attention to?

I understand that I should use Hephaestus, but I don't know how to do that if my sample contains lots of different oxides. I attached the elemental composition in this email. Most metals should be in form of oxides, or sulfates.

Any input would be highly appreciated,

Mengling

_______________________________________________ Ifeffit mailing list Ifeffit@millenia.cars.aps.anl.gov http://millenia.cars.aps.anl.gov/mailman/listinfo/ifeffit

_______________________________________________ Ifeffit mailing list Ifeffit@millenia.cars.aps.anl.gov http://millenia.cars.aps.anl.gov/mailman/listinfo/ifeffit

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"Dr. Dariusz A. Zając"

30 Sep 30 Sep

1:32 a.m.

Hi Matt, I didn't know what kind of detector is on 5-BM-D beamline and what the size of the beam is, so my answer was more general, and bases on my experience from Hasylab. I have checked now: Canberra 13-element SSD and 15x5mm2 unfocused. So, I would follow your suggestion and start with 13-element detector. Making a pellet, I suppose, will help for "broad" unfocused beam. Unfortunately I have no comparable results for PFY and TFY detection, but I have tried to measure fresco's pigments and it didnt work with 7-pixel Si(Li) Gresham but worked with PIPS diode. There is one more idea, but I do not know if this sample is crystalline or amorphous. In the first case maybe DAFS could help. I suppose it is possible at 5-BM-D... kicaj W dniu 11-09-30 01:51, Matt Newville pisze:

...

Hi Dariusz,

Thanks, those are good suggestions. I was assuming that they'd use a solid state (say 10+ element Ge) detector for concentrations at and below 10 ppm. A large diode detector might work OK -- they can often take higher total count rate at the expense of energy discrimination. I'd be happy to be shown a comparison, but my guess is that electronically removing the Fe and Compton scattering would be worth the effort for these concentrations.

--Matt

2011/9/29 "Dr. Dariusz A. Zając":

...
Dear Matt, this is very good introduction for fluorescence measurements on diluted samples... Like a tutorial... I just want to add small comments: as I understood the sample is an ash, so maybe will be possible to condense it, e.g. press it into the pellet. If there will be no possible to measure exafs (due to heavier elements), and is needed to focus on xanes, than I suggest to use non-energy dispersive detector, e.g. PIPS diode. It is very often more sensitive than regular fluorescence detectors, and can take higher count-rate. please correct me if I am wrong... kicaj

W dniu 11-09-29 17:02, Matt Newville pisze:

...
Dear Mengling,

The basic issues are: will there be enough Tl fluorescence counts in the detector, and will you be able to see a decent edge. From you spreadsheet of concentrations, the elements that stand out are: Fe and to a lesser extent Zn, and Pb.

The Fe and Zn will dominate the fluorescence getting to your detector. This hurts sensitivity to Tl because the solid-state detectors can handle a limited flux themselves (typically on the order of 100K Hz). The high Fe concentration means the Fe Kalpha will dominate the emission when you shine 12.7keV x-rays on the sample. The simple-but-effective remedy is to put aluminum foil on the detector, as aluminum will absorb Fe fluorescence (at 6.4keV) about 4x more than the Tl fluorescence (at 10.3keV). You might need a few hundred microns of aluminum foil, and may need to try a few different amounts to cut down the Fe counts sufficiently.

The other issue is Pb. The Tl L3 edge is at 12.658keV. once you hit the Pb L3 edge, at 13.1 keV, the Pb Lalpha fluorescence will dominate the Tl Lalpha fluorescence -- these lines (10.3 and 10.5 keV, respectively) are too close together to effectively filter electronically. Even well below the Pb L3 edge, you'll start to see some Pb Lalpha fluorescence. Since the Pb concentration might be 100x the Tl concentration, that would be something to look for, but there's not a lot that can be done about it. Anyway, that really only limits the EXAFS, not so much the ability to get XANES. The Tl concentrations are low, but I think that at a good APS BM line like 5-BM, getting Tl L3 XANES is just a matter of time.

Hope that helps,

--Matt

On Thu, Sep 29, 2011 at 9:39 AM, Mengling Yi Stuckman wrote:

...
Dear Ifeffit Community,

I am currently working on project "Evaluating Speciation of Thallium in Coal Fly Ash". The project was accepted by APS and we will conduct our measurement on beamline 5-BM-D.

My fly ash sample has Tl concentration ranging from 0.5ppm to 13ppm. How can I know whether the sample can generate enough photon counts if using fluorescence mode? what would be the appropriate sample preparation procedure I should follow? Is there any interference I should pay attention to?

I understand that I should use Hephaestus, but I don't know how to do that if my sample contains lots of different oxides. I attached the elemental composition in this email. Most metals should be in form of oxides, or sulfates.

Any input would be highly appreciated,

Mengling

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"Dr. Dariusz A. Zając"
Matt Newville
Mengling Yi Stuckman