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Locked Re: Skimming angle XRF- Experiment

 
Edited

.mca files for the galena encrustation.

I should have labeled the picture of the sample better- that is a mm ruler, not inches!

Geo


Locked Re: Skimming angle XRF- Experiment

 

Back to collimated beam and sensor.

Examining encrustation on corner of a galena crystal.
Galena-Encrustaion-XRF-pics.jpg


Locked Re: Skimming angle XRF- Experiment

 

"How do you control the beam angle? What accuracy can you set it to and how is that measured.

Can you run a shot with and without the detector collimator I¡¯d like to see the difference.

Dud"

Same micro sample, collimator removed from sensor, replaced by home made Kapton tape protective cap.
Here are two .mcas, one showing a full minute the other is for only 10 seconds. 30kV 15uA (reduced from 20
because?of scatter) and no collimator on the Si-PIN sensor. There may be slightly different distances to the sensor's Be window, I will have to measure to verify, but they are reasonably close.

A few things stand out, since the beam isn't passing through the card, but direct to the sample this time. Evidently there is Ca in the card stock, a blank one scanned, proves it.

Beautiful Sulphur peaks now. Galena suspected.


Re: Am241 beam collimator

 

Good idea Taray.

Geo


From: "taray singh via groups.io" <sukhjez@...>
To: [email protected]
Sent: Sunday, January 31, 2021 10:42:52 AM
Subject: [XRF] Am241 beam collimator

Hi guys?

Two common ways for Am241 housing is coaxial and converging plates?

Here is an another way I am toying round.

Using radionuclide lead pigs

I manage to squeeze 4 buttons and made a pair

The advantage is mainly when using small samples??where they can be placed very close to the Am beam
I installed iphone app to resize photo?

Taray



Am241 beam collimator

taray singh
 

Hi guys?

Two common ways for Am241 housing is coaxial and converging plates?

Here is an another way I am toying round.

Using radionuclide lead pigs

I manage to squeeze 4 buttons and made a pair

The advantage is mainly when using small samples??where they can be placed very close to the Am beam
I installed iphone app to resize photo?

Taray


Re: This Groups.io memory problems

 

Don't panic Taray, your stuff is good to retain original,becuase it shows the steps for students.? Only duplicates should be removed, or of possible reduced in size if that even applies.

George?


From: "taray singh via groups.io" <sukhjez@...>
To: [email protected]
Sent: Sunday, January 31, 2021 9:47:57 AM
Subject: Re: [XRF] This Groups.io memory problems

Geo
I think we can minimize on?sending pics ?of Mca files?
I think ?some of my??pic ?mca?files ?in the database can be deleted?
Taray




On Sunday, January 31, 2021, 10:39 PM, GEOelectronics@... wrote:

Yesterday I tried to upload some documents concerning the Tel-X-Ometer and its copper target tube generator, the whole post was rejected by the system with a warning about exceeding the free memory limits of this group. Come to find out there is only 1GB free of cost. Not much for a pictures based discussion.

So please try to limit the size of the pictures, and when replying to a post with pictures, learn to to so without repeating the pictures unless is is important to the discussion.

Now I'm going back to the beginning post and manually removing the repeated pictures to hopefully buy us some time before we have to move the XRF-PAGE2 group and archive this one. If? members can do this themselves for their own posts it would be welcomed.
Shades of our original groups on Yahoo much?

PS there is a monthly fee of $20 for an extra 9GB but I'm personally in no position to fund that for 15 groups!

Geo


Re: This Groups.io memory problems

taray singh
 

Geo
I think we can minimize on?sending pics ?of Mca files?
I think ?some of my??pic ?mca?files ?in the database can be deleted?
Taray




On Sunday, January 31, 2021, 10:39 PM, GEOelectronics@... wrote:

Yesterday I tried to upload some documents concerning the Tel-X-Ometer and its copper target tube generator, the whole post was rejected by the system with a warning about exceeding the free memory limits of this group. Come to find out there is only 1GB free of cost. Not much for a pictures based discussion.

So please try to limit the size of the pictures, and when replying to a post with pictures, learn to to so without repeating the pictures unless is is important to the discussion.

Now I'm going back to the beginning post and manually removing the repeated pictures to hopefully buy us some time before we have to move the XRF-PAGE2 group and archive this one. If? members can do this themselves for their own posts it would be welcomed.
Shades of our original groups on Yahoo much?

PS there is a monthly fee of $20 for an extra 9GB but I'm personally in no position to fund that for 15 groups!

Geo


This Groups.io memory problems

 

Yesterday I tried to upload some documents concerning the Tel-X-Ometer and its copper target tube generator, the whole post was rejected by the system with a warning about exceeding the free memory limits of this group. Come to find out there is only 1GB free of cost. Not much for a pictures based discussion.

So please try to limit the size of the pictures, and when replying to a post with pictures, learn to to so without repeating the pictures unless is is important to the discussion.

Now I'm going back to the beginning post and manually removing the repeated pictures to hopefully buy us some time before we have to move the XRF-PAGE2 group and archive this one. If? members can do this themselves for their own posts it would be welcomed.
Shades of our original groups on Yahoo much?

PS there is a monthly fee of $20 for an extra 9GB but I'm personally in no position to fund that for 15 groups!

Geo


Re: Supplements exposed :filling materials of pharmaceuticals

 

¿ªÔÆÌåÓý

Am is not cleaner than a tube with all the Np interference. A tube allows you to target the K edges and functions to selectively target a Z range of elements. To do that with a isotopic source you need to change sources Am for high Z, Cd? or Co 57 for the lower Z¡¯s. The choice of a sealed source is targeted for the elements of interest same for a tube anode. There are advantages of using a sealed source with monochromatic energy but that is usually application specific like looking for layers of Pb paint with Cd-109.? Sealed sources are in the mCi category to get the intensity needed for a good count while tubes are dial-dose.

Dud

?

From: [email protected] [mailto:[email protected]] On Behalf Of GEOelectronics@...
Sent: Saturday, January 30, 2021 10:27 AM
To: [email protected]
Subject: Re: [XRF] Supplements exposed :filling materials of pharmaceuticals

?

Taray I'm experimenting with a tube generator for education, and that's the "beam". Otherwise I use the AmX8 extensively. It is still the best way from a number of standpoints, and I will continue trying to improve the arrangement. The 59.5 is higher than 50kV max on these small tube generators, and infinitely "cleaner" than a tube.

?

Unfortunately the AmX8 is not as powerful as tube, so the skimming is not working as well. Pic shows the same old sources that started this whole thing, each with only 8 pcs. More or stronger does not help much, getting the rays in the right positionand angle s more important.

?

?

?

----- Original Message -----
From: taray singh via groups.io <sukhjez@...>
To: [email protected]
Sent: Sat, 30 Jan 2021 11:41:49 -0500 (EST)
Subject: Re: [XRF] Supplements exposed :filling materials of pharmaceuticals

?


Geo



This thing is very sensitive??indeed

The size,distance??and??Z of??any mount or base matters??besides the Am button arrangement?

?I have removed all supporting clips now

?I am using an old cardboard box as platform??so that it??is sufficiently far??from my ceramic tiles My tiles were shooting Zn peaks. I hope any recycling stuff???from the box is not causing any contaminations either?

My room is ?small and?cramped up.

So I use the floor instead??as a base.

I think it appears to be better now

Anyway I am still??seeing Fe in my aspirin pills?

No I have tried any Fe pills or foodstuff.

Very interesting using such small amounts??

with small sensor windows?

Are u using Am or X ray?

Nice if you??could??show us the setup??once you get it going.

?

Taray





On Saturday, January 30, 2021, 10:59 PM, GEOelectronics@... wrote:

Thanks for that update Taray.

Your system is very sensitive to Fe.
Have you tried Iron supplement pills or iron-added cereal food?

I tried calcium pills before but no luck, now with the new experimental arrangement here, I'll do so again to see.

The other day I tried the 1gram of Eu powder again, it was very clear to see, but the hole in the sensor is reduced to only 1mm diameter, so I transferred 25mg of the Eu3O2 powder to another plastic baggie, it also tested just fine. Then I stuck a flat wooden stick into the 25mg powder and tested the tiny amount that stuck to the end (maybe .0.005g at most), and it read fine too.

Geo

?

?

?

?

?

?

?


Locked Re: Skimming angle XRF- Experiment

 

Randall said: "Somehow, I had the impression that the exciting beam was broadside and the low, skimming angle was
from the sample shim towards the sensor."

To answer this point, yes that arrangement is what started this thread and it refers to the GERF/GEXRF = Grazing Exit XRF. That works too but is a non-starter because the wanted rays, especially the lowest energy one and in air, have too far to go the reach the sensor, which is at the edge of the sample.

Geo

----- Original Message -----
From: "Randall Buck" <rbuck@...>
To: [email protected]
Cc: [email protected]
Sent: Saturday, January 30, 2021 3:22:11 PM
Subject: Re: [XRF] Skimming angle XRF- Experiment

Nice clear photos of the source / sample / detector geometry.

Somehow, I had the impression that the exciting beam was broadside and the low, skimming angle was
from the sample shim towards the sensor.

Did I miss the explanation of why this geometry is such an attractive improvement?

Randall

PS I once made some very small pinholes in lead by casting a stainless steel wire into a thin (~3 mm) disk of lead
then pulling it out after the lead cools. The Pb doesn't (or didn't at least) alloy with the stainless.





----- Original Message -----
From: GEOelectronics@...
To: [email protected]
Sent: Sat, 30 Jan 2021 08:54:53 -0800 (PST)
Subject: Re: [XRF] Skimming angle XRF- Experiment

Mo-Re metal alloy "stamp" .002" thick.
Molybdenum-Rhenium
Skimming, tried at 2 ( 22kV@20uA ) 22kV @ 20uA then again at 15uA. Same patterns for both, the higher current just gave higher peaks.

Pictures show geometry. Beam comes up from bottom shims through the 1mm gap between the sensor collimator and the target material.

Linear display, 2 versions with appropriate gain to show the peaks of interest.


Locked Re: Skimming angle XRF- Experiment

 
Edited

This is the story of the blue rock.
I think this is from the Blanchard mine from a field trip there (many thanks to our hosts, the NM Rock and Mineral Club who have the patent on that mine).
.
It is an interesting rock full of all kinds of minerals and elements.
At one end there is a heavy deposit of metallic looking material, XRFs as Pb, so
probably Galena according to the book.
A piece of the metallic stuff broke off as seen in the first picture.
This small piece was going to be the next target tested.

Blue-Rock-small.jpg

One method to analyze smaller samples liken this is the stick them on a small disk of card-stock cardboard with double sided tape. I must have pressed it onto the tape too hard with the tweezers, resulting of just a tiny flake breaking off and sticking to the tape. Not much more than a smudge really but shiny like metal so but the tape was ruined, so the choices were throw that away and make a new sample, or test it just for the heck of it.

Someone on this group always said "test everything", so why not.

Set up for skimming angle, 30kV 20uA 30 then 60 seconds. The samples is smaller than the hole in the collimator on the sensor, and the beam is only 1mm diameter, so getting things lined up was a problem. Turning the sample around backwards gave me a better idea where it was on the card, since it was a bit off center, so the beam now comes through the back and the XRF goes out the back through the tape and the card into the 1mm hole to the sensor.



And the results (.mca attached).- what do you think, Galena?
Geo

30kV-20uA-60s-Si-PIN-W-Coll.-flake-Mineral_from-Blue-Rock-notes.jpg


Re: Supplements exposed :filling materials of pharmaceuticals

 

Pic of AmX8 on Si-PIN with the tungsten collimator still attached and results. The target was a pure silver stamp, pressed against the front of the RapCap.

22.2Degree-AmX8-Si-PIN-W-Collimator-Ag-stamp-small-combined.jpg




Re: Supplements exposed :filling materials of pharmaceuticals

 

Taray I'm experimenting with a tube generator for education, and that's the "beam". Otherwise I use the AmX8 extensively. It is still the best way from a number of standpoints, and I will continue trying to improve the arrangement. The 59.5 is higher than 50kV max on these small tube generators, and infinitely "cleaner" than a tube.

Unfortunately the AmX8 is not as powerful as tube, so the skimming is not working as well. Pic shows the same old sources that started this whole thing, each with only 8 pcs. More or stronger does not help much, getting the rays in the right positionand angle s more important.



----- Original Message -----
From: taray singh via groups.io <sukhjez@...>
To: [email protected]
Sent: Sat, 30 Jan 2021 11:41:49 -0500 (EST)
Subject: Re: [XRF] Supplements exposed :filling materials of pharmaceuticals


Geo

This thing is very sensitive??indeed

The size,distance??and??Z of??any mount or base matters??besides the Am button arrangement?

?I have removed all supporting clips now

?I am using an old cardboard box as platform??so that it??is sufficiently far??from my ceramic tiles My tiles were shooting Zn peaks. I hope any recycling stuff???from the box is not causing any contaminations either?

My room is ?small and?cramped up.

So I use the floor instead??as a base.

I think it appears to be better now

Anyway I am still??seeing Fe in my aspirin pills?

No I have tried any Fe pills or foodstuff.

Very interesting using such small amounts??

with small sensor windows?

Are u using Am or X ray?

Nice if you??could??show us the setup??once you get it going.


Taray




On Saturday, January 30, 2021, 10:59 PM, GEOelectronics@... wrote:

Thanks for that update Taray.

Your system is very sensitive to Fe.
Have you tried Iron supplement pills or iron-added cereal food?

I tried calcium pills before but no luck, now with the new experimental arrangement here, I'll do so again to see.

The other day I tried the 1gram of Eu powder again, it was very clear to see, but the hole in the sensor is reduced to only 1mm diameter, so I transferred 25mg of the Eu3O2 powder to another plastic baggie, it also tested just fine. Then I stuck a flat wooden stick into the 25mg powder and tested the tiny amount that stuck to the end (maybe .0.005g at most), and it read fine too.

Geo








Locked Re: Skimming angle XRF- Experiment

 

Mo-Re metal alloy "stamp" .002" thick.
Molybdenum-Rhenium
Skimming, tried at 222kV @ 20uA then again at 15uA. Same patterns for both, the higher current just gave higher peaks.

Pictures show geometry. Beam comes up from bottom shims through the 1mm gap between the sensor collimator and the target material.

Linear display, 2 versions with appropriate gain to show the peaks of interest.
TXRF-.002-Mo-Re-120s-22kV-20uA-notes1-small.jpg

TXRF-.002-Mo-Re-120s-22kV-20uA-notes3A-small.jpg







Setup-small.jpg


Gap.jpg


Re: Supplements exposed :filling materials of pharmaceuticals

taray singh
 

Geo

This thing is very sensitive??indeed

The size,distance??and??Z of??any mount or base matters??besides the Am button arrangement?

?I have removed all supporting clips now

?I am using an old cardboard box as platform??so that it??is sufficiently far??from my ceramic tiles My tiles were shooting Zn peaks. I hope any recycling stuff???from the box is not causing any contaminations either?

My room is ?small and?cramped up.

So I use the floor instead??as a base.

I think it appears to be better now

Anyway I am still??seeing Fe in my aspirin pills?

No I have tried any Fe pills or foodstuff.

Very interesting using such small amounts??

with small sensor windows?

Are u using Am or X ray?

Nice if you??could??show us the setup??once you get it going.


Taray




On Saturday, January 30, 2021, 10:59 PM, GEOelectronics@... wrote:

Thanks for that update Taray.

Your system is very sensitive to Fe.
Have you tried Iron supplement pills or iron-added cereal food?

I tried calcium pills before but no luck, now with the new experimental arrangement here, I'll do so again to see.

The other day I tried the 1gram of Eu powder again, it was very clear to see, but the hole in the sensor is reduced to only 1mm diameter, so I transferred 25mg of the Eu3O2 powder to another plastic baggie, it also tested just fine. Then I stuck a flat wooden stick into the 25mg powder and tested the tiny amount that stuck to the end (maybe .0.005g at most), and it read fine too.

Geo


Re: Supplements exposed :filling materials of pharmaceuticals

 

Thanks for that update Taray.

Your system is very sensitive to Fe.
Have you tried Iron supplement pills or iron-added cereal food?

I tried calcium pills before but no luck, now with the new experimental arrangement here, I'll do so again to see.

The other day I tried the 1gram of Eu powder again, it was very clear to see, but the hole in the sensor is reduced to only 1mm diameter, so I transferred 25mg of the Eu3O2 powder to another plastic baggie, it also tested just fine. Then I stuck a flat wooden stick into the 25mg powder and tested the tiny amount that stuck to the end (maybe .0.005g at most), and it read fine too.

Geo


Re: Supplements exposed :filling materials of pharmaceuticals

taray singh
 
Edited


I repeated the generic clopidogrel tablets

This time I crushed??them??to make??it homogeneous and a longer count time

Chose a??linear scale to make it. proportional .

This time only Fe is seen?
But this peak is possibly a contamination which I have corrected?
I have been having a string of Fe lately?
So I checked out an Fe clip holding Am disc was the culprit

So??this generic seems ok for use. .

Today¡¯s pandemic there is possibility of compromise in drug quality?

Generics do tend to??have some ¡°inferiority¡± to the original??but the price is cheaper?

But this does not necessarily mean they have harmful impurities?

But I will careful about??cheap generics from India or China

Only way to be sure of impurities is to do some home or lab test from time to time as batches may differ in quality?

Somebody once said

?

Everyone is entitled to his own opinion but not his own facts

TarayInline image

?

?




On Friday, January 29, 2021, 7:50 AM, taray singh via groups.io <sukhjez@...> wrote:

Dud

I too have some difficulty differentiating generics from original .

I rely??on big company names ,price and country of manufacture.

India and China famous for cheap generics .

?

?The weight fraction can be estimated in the low mg/kg-range??like in PDE limits but a poisonous ingredient in a pill is surprising and should be avoided .On top of that is coming from the filler to make it marketable.

Paracelsus law of dose related toxicity should??not be applied to tablets in my opinion.

They can find an alternative filler material or something.

Anyway I did a quick scan on some generic aspirin.There was no high Ca peak .Only Fe stood?

Anyway a longer scan need to be done with proper sample preparation?

Taray





On Friday, January 29, 2021, 4:07 AM, Dude <dfemer@...> wrote:

Very interesting on the aspirin Both have about the same Rh but the Ca is way different, amongst other things.? I may have to try this although the levels may be below my delectability. I have some Colpidogrel I¡¯ll try as well.

How do I determine generic from big boy stuff?

Dud

?https://www.agilent.com/cs/library/applications/5991-8337EN_usp_233_icpoes_application.pdf

?

From: [email protected] [mailto:[email protected]] On Behalf Of taray singh via groups.io
Sent: Wednesday, January 27, 2021 10:27 PM
To: [email protected]
Subject: Re: [XRF] Supplements exposed :filling materials of pharmaceuticals

?

Hi guys
Pharmaceuticals have some active ingredients but their main components? are fillers.
These? fillers have some functions which? are not? necessarily therapeutic but can influence the tolerance to a drug.
But they can be? ?used for identification of manipulated products? such as presence? of inorganic compounds? especially in some generics.
As a reference I have provided a micro xrf lab results of a sample of Aspirin Baeyer original and a generic.
The generic filler has more inorganic compounds? compared to the original
Pb is astonishingly present in the generic
Unfortunately Pb residual peaks makes it difficult to make an? analysis regarding the presence of lead with Am setup
Here I am using generic form of clopidogrel a common antiplatelet medication? better? known as Plavix
My sample is a few tablets in a polyethylene? container.
Ideally should be ground to a flat sheet for xrf
Anyway my xrf show peaks of Ti? and? Fe like the lab results
Best stay away from generics for long term usage drugs
Taray

?

?
?


Wavelength Dispersive X-Ray Fluorescence Spectrometer (WDXRF Spectrometer)

 

Up until now, the main subject being discussed on this group has been technically called ED-XRF. The ED is for energy dispersive. Specifically simultaneous ED, since the excitation produces a spectrum of electron shell transition energies, from which we derive the individual energy peaks all at the same time with our sensor. There is no reason in the world that an enterprising young amateur scientist couldn't do essentially the same thing manually, using a very simple SCA (single channel analyzer), analyzing the important energy peaks one step at a time.



In this thread we will explore and discuss yet another? manual sequential method called WD-XRF for Wavelength Dispersive-XRF. in which we can analyze crystal structures and have better access to the lowest energy element's identity.

Have fun,
Geo



Re: Supplements exposed :filling materials of pharmaceuticals

taray singh
 

Dud

I too have some difficulty differentiating generics from original .

I rely??on big company names ,price and country of manufacture.

India and China famous for cheap generics .


?The weight fraction can be estimated in the low mg/kg-range??like in PDE limits but a poisonous ingredient in a pill is surprising and should be avoided .On top of that is coming from the filler to make it marketable.

Paracelsus law of dose related toxicity should??not be applied to tablets in my opinion.

They can find an alternative filler material or something.

Anyway I did a quick scan on some generic aspirin.There was no high Ca peak .Only Fe stood?

Anyway a longer scan need to be done with proper sample preparation?

Taray





On Friday, January 29, 2021, 4:07 AM, Dude <dfemer@...> wrote:

Very interesting on the aspirin Both have about the same Rh but the Ca is way different, amongst other things.? I may have to try this although the levels may be below my delectability. I have some Colpidogrel I¡¯ll try as well.

How do I determine generic from big boy stuff?

Dud

?https://www.agilent.com/cs/library/applications/5991-8337EN_usp_233_icpoes_application.pdf

?

From: [email protected] [mailto:[email protected]] On Behalf Of taray singh via groups.io
Sent: Wednesday, January 27, 2021 10:27 PM
To: [email protected]
Subject: Re: [XRF] Supplements exposed :filling materials of pharmaceuticals

?

Hi guys
Pharmaceuticals have some active ingredients but their main components? are fillers.
These? fillers have some functions which? are not? necessarily therapeutic but can influence the tolerance to a drug.
But they can be? ?used for identification of manipulated products? such as presence? of inorganic compounds? especially in some generics.
As a reference I have provided a micro xrf lab results of a sample of Aspirin Baeyer original and a generic.
The generic filler has more inorganic compounds? compared to the original
Pb is astonishingly present in the generic
Unfortunately Pb residual peaks makes it difficult to make an? analysis regarding the presence of lead with Am setup
Here I am using generic form of clopidogrel a common antiplatelet medication? better? known as Plavix
My sample is a few tablets in a polyethylene? container.
Ideally should be ground to a flat sheet for xrf
Anyway my xrf show peaks of Ti? and? Fe like the lab results
Best stay away from generics for long term usage drugs
Taray


Re: Supplements exposed :filling materials of pharmaceuticals

 

¿ªÔÆÌåÓý

Very interesting on the aspirin Both have about the same Rh but the Ca is way different, amongst other things.? I may have to try this although the levels may be below my delectability. I have some Colpidogrel I¡¯ll try as well.

How do I determine generic from big boy stuff?

Dud

?https://www.agilent.com/cs/library/applications/5991-8337EN_usp_233_icpoes_application.pdf

?

From: [email protected] [mailto:[email protected]] On Behalf Of taray singh via groups.io
Sent: Wednesday, January 27, 2021 10:27 PM
To: [email protected]
Subject: Re: [XRF] Supplements exposed :filling materials of pharmaceuticals

?

Hi guys
Pharmaceuticals have some active ingredients but their main components? are fillers.
These? fillers have some functions which? are not? necessarily therapeutic but can influence the tolerance to a drug.
But they can be? ?used for identification of manipulated products? such as presence? of inorganic compounds? especially in some generics.
As a reference I have provided a micro xrf lab results of a sample of Aspirin Baeyer original and a generic.
The generic filler has more inorganic compounds? compared to the original
Pb is astonishingly present in the generic
Unfortunately Pb residual peaks makes it difficult to make an? analysis regarding the presence of lead with Am setup
Here I am using generic form of clopidogrel a common antiplatelet medication? better? known as Plavix
My sample is a few tablets in a polyethylene? container.
Ideally should be ground to a flat sheet for xrf
Anyway my xrf show peaks of Ti? and? Fe like the lab results
Best stay away from generics for long term usage drugs
Taray