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Re: Stainless Steel XRF

 

开云体育

Geo,

Why is there ?4.8mm of Al attenuator in the beam path? ?What is the no collimated diameter of the micro-focus beam on the target? Is it well aligned with the 1mm collimator, if it’s not you’ll have ?a lot of attenuation.? Collimation usually uses 2 ?separated collimators and sometimes one on the detector. ?Start simple, no collimator, no attenuators. Look at the beam diameter at the target plane. Set up the collimation to get the beam diameter you want at the target plane. ?Then move the Detector close to the target say about 1 – 2cm. ?Take a shot using the lowest beam current and look at Dead Time. You should be able to count at 40Kcps and have good resolution and count time.? Play with the beam current. Play with Detector distance to target.

Your comment “…allows the sensor to be considerably close to the center of the chamber. Not that? it maters very much” ?What is considerably closer? It matters very much. The beam will expose a small circle on the target that will fluoresce over a solid angle. The flux in is proportional to the flux out. The percentage of that signal your detector will get is directly dependent on the distance from the target and that solid angle. Close up its 1/r, at a distance it falls as 1/r2.? Remember the time distance shielding thing

?Do a sensitivity analysis. What gets the best signal? What changes things the most? – where do I optimize my effort? Is it Distance, geometric angle between beam and detector, collimation, need for attenuator, what size beam spot do I want on the target, what s that get me in count time etc.

The problem here is not the difference between a SDD and a SI-PIN it’s the set up geometry and the shield system limiting you to very poor performance.

Dud

KK7IF

?

?

From: [email protected] [mailto:[email protected]] On Behalf Of GEOelectronics@...
Sent: Tuesday, February 4, 2020 7:32 PM
To: [email protected]
Subject: Re: [XRF] Stainless Steel XRF

?

?

Yes, the exciter flux is very low. Only 20 uA and in the beam port right now are 3 ea. 1.6mm Aluminum plates (solid) and then a 4.75mm plate with a 1mm hole in the center. I'm please with the clean patterns, even tho slow. This is a Si-PIN, not an SDD.?

?

I did machine a new part the other day that connects the Al and Pb? cylinders together, that allows the sensor to be considerably close to the center of the chamber. Not that? it maters very much, as the beam can be positioned anywhere on the floor of the chamber.

?

Also today, a trip to the garage yielded a good thick aluminum part that can be turned on the lather to make the lid-liner,

With luck, the lid will be finished tomorrow and work on the permanent collimator started.

Geo

----- Original Message -----
From: Dude <dfemer@...>
To: [email protected]
Sent: Tue, 04 Feb 2020 19:52:13 -0500 (EST)
Subject: Re: [XRF] Stainless Steel XRF

?


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Geo,

Getting only 1800 counts/sec ?in 600 sec is saying something is
not quite right with the setup. Not separating the Fe and Ni Kb and Ka is also
not right but may? be related to the low count rate. Before you go any further
find out why you’re getting the low count rate. This spectra should come in in ?30
sec count. ?I suspect the beam flux is too low (what’s the collimator diameter
and where is the micro-focus point?) and if you haven’t moved the detector
closer to the target ?that may be the problem as well.? Get rid of the lead shield
setup and set up the geometry by hand without it (but keeping ?shielding between
you and it). Play around getting an optimal geometry and beam current. Start by
getting the detector closer to the target.? I’d think running ?a test with and
without the plastic cap on the low energy end would be interesting test to see
as well. Use a Si target.

Dud

Sent: Tuesday, February
4, 2020 2:02 PM
To: [email protected]
Subject: [XRF] Stainless Steel XRF

?

Baby steps- a 304 stainless bolt from the shop.


Geo

?

?

?

?

?


Re: Stainless Steel XRF

 


Yes, the exciter flux is very low. Only 20 uA and in the beam port right now are 3 ea. 1.6mm Aluminum plates (solid) and then a 4.75mm plate with a 1mm hole in the center. I'm please with the clean patterns, even tho slow. This is a Si-PIN, not an SDD.?

I did machine a new part the other day that connects the Al and Pb? cylinders together, that allows the sensor to be considerably close to the center of the chamber. Not that? it maters very much, as the beam can be positioned anywhere on the floor of the chamber.

Also today, a trip to the garage yielded a good thick aluminum part that can be turned on the lather to make the lid-liner,
With luck, the lid will be finished tomorrow and work on the permanent collimator started.
Geo

----- Original Message -----
From: Dude <dfemer@...>
To: [email protected]
Sent: Tue, 04 Feb 2020 19:52:13 -0500 (EST)
Subject: Re: [XRF] Stainless Steel XRF

Geo,

Getting only 1800 counts/sec ?in 600 sec is saying something is
not quite right with the setup. Not separating the Fe and Ni Kb and Ka is also
not right but may? be related to the low count rate. Before you go any further
find out why you’re getting the low count rate. This spectra should come in in ?30
sec count. ?I suspect the beam flux is too low (what’s the collimator diameter
and where is the micro-focus point?) and if you haven’t moved the detector
closer to the target ?that may be the problem as well.? Get rid of the lead shield
setup and set up the geometry by hand without it (but keeping ?shielding between
you and it). Play around getting an optimal geometry and beam current. Start by
getting the detector closer to the target.? I’d think running ?a test with and
without the plastic cap on the low energy end would be interesting test to see
as well. Use a Si target.

Dud

Sent: Tuesday, February
4, 2020 2:02 PM
To: [email protected]
Subject: [XRF] Stainless Steel XRF

?

Baby steps- a 304 stainless bolt from the shop.


Geo







Re: Stainless Steel XRF

 

开云体育

Geo,

Getting only 1800 counts/sec ?in 600 sec is saying something is not quite right with the setup. Not separating the Fe and Ni Kb and Ka is also not right but may? be related to the low count rate. Before you go any further find out why you’re getting the low count rate. This spectra should come in in ?30 sec count. ?I suspect the beam flux is too low (what’s the collimator diameter and where is the micro-focus point?) and if you haven’t moved the detector closer to the target ?that may be the problem as well.? Get rid of the lead shield setup and set up the geometry by hand without it (but keeping ?shielding between you and it). Play around getting an optimal geometry and beam current. Start by getting the detector closer to the target.? I’d think running ?a test with and without the plastic cap on the low energy end would be interesting test to see as well. Use a Si target.

Dud

Sent: Tuesday, February 4, 2020 2:02 PM
To: [email protected]
Subject: [XRF] Stainless Steel XRF

?

Baby steps- a 304 stainless bolt from the shop.

Geo

304-Bolt-Scan-XRF-Pub.png


Re: Ken's "Mystery Wire"

 

Thanks Randall! This is great fun and it's nice to be able to watch the peaks build real-time. It seems the best thing is to do is take a reading at 60 seconds, 300 seconds and 600 seconds for the record, saving each for futu re reference.

Today all of my moly samples (stamps I call them they are the size of a letter stamp) -were tested, holy cow the sheet metal ones are really loaded with minor amendments and contamination not visible on NaI(Tl) (great for moly peaks for cal tho, even on Si-PIN). Also testing the Ni-Mo alloys, pretty interesting.

George

----- Original Message -----
From: Randall Buck <rbuck@...>
To: [email protected]
Cc: [email protected]
Sent: Mon, 03 Feb 2020 13:37:22 -0500 (EST)
Subject: Re: [XRF] Ken's "Mystery Wire"


Very nice bit of detective work,
Congratulations, Geo.

Randall



----- Original Message -----
From: GEOelectronics@...
To: [email protected]
Sent: Sun, 02 Feb 2020 08:15:07 -0800 (PST)
Subject: Re: [XRF] Ken's "Mystery Wire"

Right now the chamber has a 1" thick aluminum lid, topped with several thin lead "blankets", a flexible shielding material. No leakage out of the top but more importantly no Pb XRF from the old lid shows up in the scan. From this I can design a new lid.

Tweaking the kV and uA, for the mystery wire, concentrating on a starting point,
we can now ID low Ni/ Chrome Moly Steel in 20 seconds. Next week
I will start the hunt for some know SS alloy samples at the local steel yard.
Bottom line, comparing to a known source is always best and easiest, not that they are likely to have any of this particular material on hand.

Ken do you have a 1 gram piece for Dudley?

Folks, would we call this Chrome-Moly Steel, with alloy to be determined later?

Geo


Re: Ken's "Mystery Wire"

 

Very nice bit of detective work,
Congratulations, Geo.

Randall

----- Original Message -----
From: GEOelectronics@...
To: [email protected]
Sent: Sun, 02 Feb 2020 08:15:07 -0800 (PST)
Subject: Re: [XRF] Ken's "Mystery Wire"

Right now the chamber has a 1" thick aluminum lid, topped with several thin lead "blankets", a flexible shielding material. No leakage out of the top but more importantly no Pb XRF from the old lid shows up in the scan. From this I can design a new lid.

Tweaking the kV and uA, for the mystery wire, concentrating on a starting point,
we can now ID low Ni/ Chrome Moly Steel in 20 seconds. Next week
I will start the hunt for some know SS alloy samples at the local steel yard.
Bottom line, comparing to a known source is always best and easiest, not that they are likely to have any of this particular material on hand.

Ken do you have a 1 gram piece for Dudley?

Folks, would we call this Chrome-Moly Steel, with alloy to be determined later?

Geo


2 Stage Exciters

 

There is a scheme where the main exciter, say an X-Ray tube or isotope, excites an intermediate target, causing XRF rays, which in turn are used to excite the main target. This method allows the conversion of a noisy exciter source to a different energy level (K and L lines of the intermediate target) and make the final ray much cleaner.

I've personally tried this on the bench and it does work, but would like to scale it up, just to see.

Here's a picture found online showing graphically the arrangement, pretty basic stuff.


Geo>K0FF


Re: bassetite Si-PIN

 

yeah here it is. Ka1 Kb1

together. Now to try to merge some L lines in there.

Ka_Kb-Metals.png


Re: bassetite Si-PIN

 

didn't you send me one before that was combined> I'm looking for it now as a place to start.

----- Original Message -----
From: Dude <dfemer@...>
To: [email protected]
Sent: Sun, 02 Feb 2020 17:54:02 -0500 (EST)
Subject: Re: [XRF] bassetite Si-PIN

I’m not sure what the Amptek look up library can handle. It seems
it only is set up for a Ka Kb or La Lb can ?we mix K’s and L’s ?in there as
well and have it report correctly?? Inquiring minds want to know.

Dud

?

From: [email protected]
[mailto:[email protected]] On Behalf Of GEOelectronics@...
Sent: Sunday, February 2, 2020 2:27 PM
To: [email protected]
Subject: Re: [XRF] bassetite Si-PIN

?

On Sun, Feb 2, 2020 at 04:20 PM, Dude wrote:

We need to check and fix these libraries.

I agree, at a minimum a library of the Periodic Table
elements, one or two at a time well separated with no overlapping peaks, with
all 4 lines, Ka, Kb, La, Lb.


Geo







Re: bassetite Si-PIN

 

开云体育

I’m not sure what the Amptek look up library can handle. It seems it only is set up for a Ka Kb or La Lb can ?we mix K’s and L’s ?in there as well and have it report correctly?? Inquiring minds want to know.

Dud

?

From: [email protected] [mailto:[email protected]] On Behalf Of GEOelectronics@...
Sent: Sunday, February 2, 2020 2:27 PM
To: [email protected]
Subject: Re: [XRF] bassetite Si-PIN

?

On Sun, Feb 2, 2020 at 04:20 PM, Dude wrote:

We need to check and fix these libraries.

I agree, at a minimum a library of the Periodic Table elements, one or two at a time well separated with no overlapping peaks, with all 4 lines, Ka, Kb, La, Lb.

Geo


Re: bassetite Si-PIN

 

On Sun, Feb 2, 2020 at 04:20 PM, Dude wrote:
We need to check and fix these libraries.
I agree, at a minimum a library of the Periodic Table elements, one or two at a time well separated with no overlapping peaks, with all 4 lines, Ka, Kb, La, Lb.

Geo


Re: bassetite Si-PIN

 

开云体育

Geo,

The Rb you’re looking at , sorry, the computer is looking at is U Ka at 13.6, ?Rb has a Ka of 13.4 they can get confused if the ROI is not selected correctly. However in this case the Amptek Ka library doesn’t have a listing for U Ka so it’s never reported.? We need to check and fix these libraries.

Here’s some sage advice; The computer is not your friend, it hates you and everything you stand for because you’re smarter than it is. Its crafty – It has a Critical Need Detector and it’ll wait for the best possible moment to get its revenge. To avoid this DO EVERTHING YOURSELF.

?

To interpret spectra? first look at it. Good well defined peaks or Noisy? Rerun it for a longer count

Then start at the low energy side and manually set ROI’s for each peak. For each peak find its peak energy and the look up in the x-ray table to determine what are the possible elements. Then look the for the Kb or Lb and confirm what you are looking at. Ka to Kb ratio is abt 5:1 La to ?Lb ?is 1:1 or so. If it doesn’t have a brother then it’s not a positive ID just unconfirmed.? Low Z elements won’t have any L peaks only K. Middle Z will have both and High Z will have L and possibly K depending on excitation energy. ?Some peaks are going to be good peaks others will be unknowns. The unknowns are artifacts and will include the sum, escape, ?backscatter, Compton, Rayleigh and merged peaks that are there just to harass and humble you.

In each case it’s up to you to interpret the data, the computer picks will 100% get you into trouble without verification .

Do not preconceive anything. For the Theromino and PXRF ?crowd - Don’t set any element lines on the screen. YOU set them as you ID an element. Don’t bias yourself. Believe nothing verify everything.? Just because you always had a Pb line set up doesn’t mean this time it’s not an As.? If you can’t figure it out without help lines you’re using a faulty interpretation model that will surely get you in trouble.? BTW ?the Garbage-In-Garbage- Out phrase was actually based on computer XFR interpretations ?not on the computer models it is usually attributed to.

XRF interpretation is not quick or easy but It’s very satisfying…when it works

Dud

?

?

From: [email protected] [mailto:[email protected]] On Behalf Of GEOelectronics@...
Sent: Sunday, February 2, 2020 8:28 AM
To: [email protected]
Subject: Re: [XRF] bassetite Si-PIN

?

Update- Bassetite, Si-PIN in new chamber, 10mins 40kV/30uA.

Does Bassetite normally contain Rb and Sr?

I'll crank it up and look at the lanthanides next..

Geo>K0FF


Re: Ken's "Mystery Wire"

 

Here's the 600s scan after doing the work on the beam and lid.Take a good look at Te and Ru lines, can those be real?

600s-Scan-Chrome-Moly-Steel-.jpg


Re: Ken's "Mystery Wire"

 

sounds like a great plan, but they count the seconds on their X-Ray tube and won't do any favors......Unless maybe I say I have 500 pounds of "this material" what is it worth?

----- Original Message -----
From: Dude <dfemer@...>
To: [email protected]
Sent: Sun, 02 Feb 2020 14:20:13 -0500 (EST)
Subject: Re: [XRF] Ken's "Mystery Wire"

Geo,

My system cal uses a 316 SS disk. Take the wire with you and see if
they have a xrf metal analyzer and get an ID that way.

Dud

?

From: [email protected]
[mailto:[email protected]] On Behalf Of GEOelectronics@...
Sent: Sunday, February 2, 2020 8:15 AM
To: [email protected]
Subject: Re: [XRF] Ken's "Mystery Wire"

?

Right now the chamber has a 1" thick aluminum lid,
topped with several thin lead "blankets", a flexible shielding
material. No leakage out of the top but more importantly no Pb XRF from the old
lid shows up in the scan. From this I can design a new lid.


Tweaking the kV and uA, for the mystery wire, concentrating on a starting
point,?

we can now ID low Ni/ Chrome Moly Steel in 20 seconds. Next week?

I will start the hunt for some know SS alloy samples at the local steel
yard.?

Bottom line, comparing to a known source is always best and easiest, not that
they are likely to have any of this particular material on hand.


Ken do you have a 1 gram piece for Dudley?


Folks, would we call this Chrome-Moly Steel, with alloy to be determined later?



Geo







Re: Ken's "Mystery Wire"

 

开云体育

Geo,

Attached is a manually selected ROI showing the Cr, Fe, Mo, and the missing Ni. ?Using auto generated ROI computer picks usually are not very helpful and in the end its probably best to set your own using a quasi-heuristic approach (by eye-ball) for the ROI’s.

Note that these peaks are noisy and under sampled with the largest peak, Fe, having only 212 counts in it for a 20 sec count.? The count rate is 2306 cps which is slow for this detector which can handle a much higher count rate. ?For your 4.8 usec peaking time you should be able get up to 50,000 cps.? To do that try a couple of things, ?get the detector closer to the target, increase the beam current and optimize the collimator’s beam diameter. ?I suspect? the large standoff distance of the detector may be the most sensitive to the problem.?

The Cal Check.bmp ?attachment is a 30 sec 50 kV shot of a 316 SS calibration disk resulting in a count rate of 31,861 cps.? Note the Fe peak is well defined and has a 1909 count peak.

Dud

KK7IF

?

?

From: [email protected] [mailto:[email protected]] On Behalf Of GEOelectronics@...
Sent: Sunday, February 2, 2020 8:15 AM
To: [email protected]
Subject: Re: [XRF] Ken's "Mystery Wire"

?

Right now the chamber has a 1" thick aluminum lid, topped with several thin lead "blankets", a flexible shielding material. No leakage out of the top but more importantly no Pb XRF from the old lid shows up in the scan. From this I can design a new lid.

Tweaking the kV and uA, for the mystery wire, concentrating on a starting point,?
we can now ID low Ni/ Chrome Moly Steel in 20 seconds. Next week?
I will start the hunt for some know SS alloy samples at the local steel yard.?
Bottom line, comparing to a known source is always best and easiest, not that they are likely to have any of this particular material on hand.

Ken do you have a 1 gram piece for Dudley?

Folks, would we call this Chrome-Moly Steel, with alloy to be determined later?


Geo
20s-Scan-Chrome-Moly-Steel-.png


Re: Ken's "Mystery Wire"

 

开云体育

Geo,

My system cal uses a 316 SS disk. Take the wire with you and see if they have a xrf metal analyzer and get an ID that way.

Dud

?

From: [email protected] [mailto:[email protected]] On Behalf Of GEOelectronics@...
Sent: Sunday, February 2, 2020 8:15 AM
To: [email protected]
Subject: Re: [XRF] Ken's "Mystery Wire"

?

Right now the chamber has a 1" thick aluminum lid, topped with several thin lead "blankets", a flexible shielding material. No leakage out of the top but more importantly no Pb XRF from the old lid shows up in the scan. From this I can design a new lid.

Tweaking the kV and uA, for the mystery wire, concentrating on a starting point,?
we can now ID low Ni/ Chrome Moly Steel in 20 seconds. Next week?
I will start the hunt for some know SS alloy samples at the local steel yard.?
Bottom line, comparing to a known source is always best and easiest, not that they are likely to have any of this particular material on hand.

Ken do you have a 1 gram piece for Dudley?

Folks, would we call this Chrome-Moly Steel, with alloy to be determined later?


Geo
20s-Scan-Chrome-Moly-Steel-.png


Re: bassetite Si-PIN

 

Seems shorter runs with higher HV and lower uA make a better scan, like Dudley mentioned about pileup. On this one, set the HV all the way up, brought the uA up until deadtime started showing, set uA for 2.5% D.T.

Displayed in LOG mode, this is way too complicated to analyze by eye, I think. Analysis was with Ka1 library only, will do again for Kb, La, Lb when time allows. Several elements do show both K and L peaks. As much setup data as possible? included for the record.
,mca attached.

Bassetite-Analysis_Setup-53kV-40uA-200s-02FEB2020-LOWERS.png

Bassetite-Analysis_Setup-53kV-40uA-200s-02FEB2020-UPPERS.png
Now I am thinking of leaving this set up and doing further experiments, and will be glad to try to analyze samples from members for practice.

Geo>K0FF


Re: bassetite Si-PIN

 

Update- Bassetite, Si-PIN in new chamber, 10mins 40kV/30uA.

Does Bassetite normally contain Rb and Sr?

I'll crank it up and look at the lanthanides next..

Geo>K0FF


Re: Ken's "Mystery Wire"

 

Right now the chamber has a 1" thick aluminum lid, topped with several thin lead "blankets", a flexible shielding material. No leakage out of the top but more importantly no Pb XRF from the old lid shows up in the scan. From this I can design a new lid.

Tweaking the kV and uA, for the mystery wire, concentrating on a starting point,?
we can now ID low Ni/ Chrome Moly Steel in 20 seconds. Next week?
I will start the hunt for some know SS alloy samples at the local steel yard.?
Bottom line, comparing to a known source is always best and easiest, not that they are likely to have any of this particular material on hand.

Ken do you have a 1 gram piece for Dudley?

Folks, would we call this Chrome-Moly Steel, with alloy to be determined later?


Geo
20s-Scan-Chrome-Moly-Steel-.png


Re: 2020 Portable X-Ray Tube XRF Outfit.- Fine Tuning the Chamber Lid

 

The original simple lead (Pb)? lid worked great as a shield but was giving stray Pb XRF peaks to the detector.
To fine tune it, different combinations of aluminum topped with lead were tried and tested.

It's going to take a thick aluminum lining and a thinner lead top to get rid of the strays.. The picture shows the arrangement of materials that worked.

I discovered that there is leakage along the edges of the thick aluminum when used as a shield, probably from internal scattering. Therefore the final lid will have the aluminum layer a smaller diameter than the Pb top, so it can be completely surrounded by the Pb chamber wall. Perhaps I'll simply attach an thick aluminum disc to the bottom side of the existing lid.

Fine_tuning_chamber_lid-small.jpg

A 10 minute scan to record the background radiation picked up by the Si-PIN when inserted into the chamber, but no exciter present. Only two hits were recorded,? probably random Cosmic Ray Muons

Chamber-BG-small.jpg



Geo>K0FF