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XRF Wiki
Welcome to the XRF Wiki. This Wiki is a repository of information contributed by members of [email protected]. Members can view and edit the pages. The pages are currently not viewable by the public. The pages below represent a rough overview of the technology and techniques associated with X-Ray Florescence Spectroscopy as well as serving as a place for members to organize the spectra that they have contributed to the forum.?
As a starting point, the pages will be populated by information taken from member posts from the past few years - with references/attribution. Perhaps in time, these pages can be edited by members to make them more complete and less choppy. Members can also edit this page, making the structure of the content more organized.?
Pages can contain information about a particular topic, links to relevant resources (such as manuals, research papers, etc.), links to relevant forum discussions on the topic, book titles, or anything that might be useful.
What follows is very much a work in progress.
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Adding to the Wiki
For those unfamiliar with the Wiki phenomenon, it is basically a user editable encyclopedia. The idea is that there are pages with different articles, which the user can read and also choose to edit if desired. If a piece of information is incorrect, a link outdated, or the presentation choppy or unclear, the user can just click "Edit Page" at the bottom and then fix the mistake. There is also a "Page History," so if you a user were to make a mistake or maliciously destroy a page (which wouldn't happen here) an editor can come along and restore the page to a previous version.?
If you have used MediaWiki (the engine that runs behind the scene of Wikipedia.org) you will be familiar with a certain style of creating an article. There are tags that one uses to change the formatting of the parts of the article. The Wiki on Groups.io uses a different background engine and so the standard MediaWiki syntax does not apply here. Rather, the page is edited using the same tools as one would use to compose a message on the forums. If you are a programmer or someone who likes using the tagged syntax directly, you can access the underlying page source code, be activating the advanced editing toolbar (the icon with three lines on the far right of the basic toolbar) and then clicking on the source code icon <> on the far right of the Advance Editing Toolbar. You will immediately notice that the underlying source code is HTML. Most things can be done just by using the various icons, but advanced features like table can only be implemented by manually writing the source code. (Although there are website available that will generate the source code for you through a graphical interface.)
Here are some useful resources from Groups.io:?
Wiki Guide for Users and Editors
Message Composition Tips and Tricks
Overview of XRF
X-Ray Florescence vs. X-Ray Diffraction
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Hardware
This section describes the hardware used for XRF. We will describe the basic theory of operation of each stage in the processing tool chain and then present different commercial systems that are available as these systems are often integrated together.
[Editor note: General theory needs to be in an independent page separate from specific manufacturer information.
[Editor note - question: Should this be arranged by category, e.g detectors, preamps, etc or by manufacturer with the manufacturers product line on one page. Perhaps it's best to put a list of products with theory but the details of the products on a manufacture page...]
Detectors?- what's available, theory of operation, tradeoffs
Detector Cooling?- keeping detectors cool to avoid thermal noise and keeping the TEC from overheating
Preamps?- theory of operation, brief summary of what out there (and what not to do - such as trying to use a PMT preamp for a SiPIN diode...)
Pulse Processing Theory - high level overview of the stages of going from detector pulse to channel peaks on the computer
Commercial Systems - many commercial systems are integrated so it seems to make sense to present, for example all Amptek products together. [question: are their other affordable integrated systems besides Amptek?]
Amptek XRF System
Activation Sources - what do you use to make the sample fluoresce (that's within the amateur budget and doesn't require special licensing)
Software
- Device Control Software - what do you use to collect the data from the detector system
- XRF Analysis Software - what do you use to analyze the data, especially for quantitative measurements (composition percentages, thin film measurement)
- Free Software Tools
Note: there may be software packages that possess some or all of these characteristics.
Materials Spectra
Metals Spectra
Historic/Archeological Spectra
Reference Materials Spectra
Household Objects Spectra
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Resources
Videos
Articles
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Non-XRF Techniques
Gamma Spectroscopy
Raman Spectroscopy
FTIR - Fourier Transform Infrared Spectroscopy
Atomic Emission Spectroscopy
Inductively Coupled Atomic Emission Spectroscopy
Spark Emission Spectroscopy
Atomic Absorption Spectroscopy
LIBS - Laser Induced Breakdown Spectroscopy
Photoacoustic Spectroscopy
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Re: FW: [XRF] 59.5keV spectrum cleanup
I agree, and we can't expect anything below ~2keV in air, but what this shows me is with a helium atmosphere, we could have a shot at down to 1. ?I tried propane (once) and it changed things, bit of course is not practical, just as hydrogen is not practical. Vacuum is best, but at this time it's not in the cards for me. Charles have you considered XRD for your minerals? If so check out the Tel-X-Ometer unit. I have several of those waiting a turn in the counting room. The way XRD works baffles me but it seems to be a very popular mode for determining crystal structure and maybe oxidation states (?). No immediate plans to do so but have used the internal copper-target X-Ray source in it many times for other purposes. Switch selectable 20 / 30 kV at 80uA. These have an integral goniometer, and the ones I get usually have that part damaged by corrosion due to leaving salt crystals in it when stored (they are a college teaching tool). Geo ----- Original Message ----- From: Charles David Young <charlesdavidyoung@...> To: XRF <[email protected]> Sent: Fri, 30 Oct 2020 10:53:09 -0400 (EDT) Subject: Re: FW: [XRF] 59.5keV spectrum cleanup It just looks like noise to me.? I would have to see a lot more counts and reproducible runs to believe it. Charles On Fri, Oct 30, 2020 at 7:47 AM <GEOelectronics@...> wrote:
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Re: Chinese water filter analysis
Great idea on the reverse-osmosis water discharge! Test everything! Here's another great idea for collecting samples from water, a paper by? "A Sensitive XRF Screening Method for Lead in Drinking Water" Abstract A novel method for quickly and quantitatively measuring aqueous lead in drinking water has been developed. A commercially available activated carbon felt has been found to effectively capture lead from tap water, and partnered with X-Ray fluorescence (XRF) spectrometry, it provides quantitative measurement of aqueous lead in drinking water. Specifically, for a 2-liter volume of tap water, the linear range of detection was found to be from 1 ¨C 150 ppb, encompassing the current EPA limit for lead in drinking water (15 ppb). To make a reproducible and easy to use method for filtering, a 2L bottle cap with a 1.25 cm diameter hole was used for filtering. Utilizing this filtration method, 75 solutions from 0 ppb to 150 ppb lead gave a 91% sensitivity, 97% specificity, and 93% accuracy and all the misclassified samples fell between 10 and 15 ppb. This method has also proved reliable for detecting calcium as well as several other divalent metals in drinking water including copper, zinc, iron, and manganese. Note- She has tested all sorts of premade activated charcoal felt sheeting to find one that is inexpensive and yet performs very well for those heavy metals. I can send the paper by email but can't post it online. Geo ----- Original Message ----- From: taray singh via groups.io <sukhjez@...> To: [email protected] Sent: Fri, 30 Oct 2020 10:14:27 -0400 (EDT) Subject: [XRF] Chinese water filter analysis Hi guys I am interested in drinking water quality testing and most drinking water test kits are not accurate. They give positive readings on concentrated samples like sewage and not for trace elements in drinking water. So I wanted to try out this interesting Chinese? gadget. Search you tube for..?Water Electrolyzer (Quality Tester). The Most Dangerous Appliance Ever? Negative comments being dangerous? and a scam. I checked it out There are 2 pairs of electrodes A shiny aluminium and a dull? iron pair. Repeated usage caused the? iron to rust. Aluminium was confirmed? by exclusion being shiny,light,cheap and nondescript. My drinking water? sample is RO? waste water . This discharged RO waste water is about 4 times more concentrated than my tap water depending on machine cycling. Concentrated means more residue better than plain tap water for analysis. My 14 in 1test kit was basically negative? for heavy metals. I tested this RO concentrated with this Chinese toy. It produced a brownish residue as expected. Collected it and allowed it dry on cap and a tissue. This cap/tissue was analyzed with Xrf with Am241/Si pin detector. True enough like the you tubers described there is Fe from galvanic reactions. There appears to be Pb peak as well I need to repeat this test with a thicker sample? to confirm . Taray . ? |
Re: FW: [XRF] 59.5keV spectrum cleanup
It just looks like noise to me.? I would have to see a lot more counts and reproducible runs to believe it. Charles On Fri, Oct 30, 2020 at 7:47 AM <GEOelectronics@...> wrote:
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Re: FW: [XRF] 59.5keV spectrum cleanup
Ok your 4.8us. Yes I ran that too for a long time.
Here's an expanded look at the lowest energy end of that scan, with pretty arrows to point out the lowest fully resolved peak (although there is another even below that one, but this one has clear on both sides and the sides go way down... The subject is very weakly radioactive, and that low peak may not have any real meaning, but now all the peaks except the odd 1 count hits are actual peaks from something, not electronics noise. Even the lowest thing visible has a top to it. Geo |
Re: FW: [XRF] 59.5keV spectrum cleanup
I have always used 4.8uS peak time. Can you show why
you think you are resolving individual peaks down to less than 1.5 keV? Charles On Fri, Oct 30, 2020 at 6:35 AM <GEOelectronics@...> wrote:
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Chinese water filter analysis
taray singh
Hi guys
I am interested in drinking water quality testing and most drinking water test kits are not accurate. They give positive readings on concentrated samples like sewage and not for trace elements in drinking water. So I wanted to try out this interesting Chinese? gadget. Search you tube for..?Water Electrolyzer (Quality Tester). The Most Dangerous Appliance Ever? Negative comments being dangerous? and a scam. I checked it out There are 2 pairs of electrodes A shiny aluminium and a dull? iron pair. Repeated usage caused the? iron to rust. Aluminium was confirmed? by exclusion being shiny,light,cheap and nondescript. My drinking water? sample is RO? waste water . This discharged RO waste water is about 4 times more concentrated than my tap water depending on machine cycling. Concentrated means more residue better than plain tap water for analysis. My 14 in 1test kit was basically negative? for heavy metals. I tested this RO concentrated with this Chinese toy. It produced a brownish residue as expected. Collected it and allowed it dry on cap and a tissue. This cap/tissue was analyzed with Xrf with Am241/Si pin detector. True enough like the you tubers described there is Fe from galvanic reactions. There appears to be Pb peak as well I need to repeat this test with a thicker sample? to confirm . Taray . ? ![]()
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chinese water tester.mca
chinese water tester.mca
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14 in 1 kit.jpg
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Re: Si-PIN Detector PEAKING-TIME-TEST
After running the 19.2us peaking time and being satisfied with the tweaking and calibration, here are the results from a and overnight U L X-Ray test and for comparison an old similar test on the same very weakly radioactive sample using 4.8us PT (both in Gamma Spectrum Analyzer mode- not excited XRF)
The differences are subtle but real, with the clarity of large peaks and better separation on smaller peaks going to the slower peaking time. However in gross analysis, both are very accurate and would probably be equally useful for element identification purposes. Differences between the scans doesn't translate to a pretty picture, so only .mca's included here. Geo 39-0-61keV-Si-PIN_43.6kSec_10FEB2020.mca
39-0-61keV-Si-PIN_43.6kSec_10FEB2020.mca
Si-PIN-U-L_X-Ray_test_30OCT2020_45500s.mca
Si-PIN-U-L_X-Ray_test_30OCT2020_45500s.mca
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Re: FW: [XRF] 59.5keV spectrum cleanup
Thanks for that report Charles. Of the two, can you say what is the lowest peak that can be resolved and is there a difference between them?? My just finished overnight run using the Si-PIN on a weakly radioactive sample for Gamma Spec (not excited XRF) is resolving individual peaks down to less than 1.5 keV. In the Peaking Time topic thread I'll post that test @19.2us PT along with a nearly similar test done last February at 4.8us. The main difference between those seems to be both in the clarity and narrowness of the big peaks, and better performance at the lowest end going to the 19.2. Today I'll try even longer peaking times, up to 32us just for the historical record.? I think you've been using 32us and I can't fault your scans, that's for sure. Geo ----- Original Message ----- From: Charles David Young <charlesdavidyoung@...> To: XRF <[email protected]> Sent: Fri, 30 Oct 2020 08:26:25 -0400 (EDT) Subject: Re: FW: [XRF] 59.5keV spectrum cleanup I did 2 runs on a brannerite specimen.? One like normal (red) and the other with a paper adhesive label covering the buttons.? The proportions of the peaks pretty much look the same to me. Charles On Wed, Oct 28, 2020 at 11:30 AM Dude <dfemer@...> wrote:
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Re: FW: [XRF] 59.5keV spectrum cleanup
I did 2 runs on a brannerite specimen.? One like normal (red) and the other with a paper adhesive label covering the buttons.? The proportions of the peaks pretty much look the same to me. Charles On Wed, Oct 28, 2020 at 11:30 AM Dude <dfemer@...> wrote:
Amptek_DppMCA_Si-PIN_gain_9999_channels_4096 brannerite headstone Area 104 Petaca NM paper filter.mca
Amptek_DppMCA_Si-PIN_gain_9999_channels_4096 brannerite headstone Area 104 Petaca NM paper filter.mca
Amptek_DppMCA_Si-PIN_gain_9999_channels_4096 brannerite headstone Area 104 Petaca NM.mca
Amptek_DppMCA_Si-PIN_gain_9999_channels_4096 brannerite headstone Area 104 Petaca NM.mca
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ThereminoMCA_Amptek_DppMCA_Si-PIN brannerite headstone Area 104 Petaca NM.png
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Re: How about Sodium?
Ok, thanks for the Na response.
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Next? gas proportional counter in a He atmosphere? I'll take some with me in the shower,that should be enlightening. Randall ----- Original Message -----
From: Dude <dfemer@...> To: [email protected] Sent: Wed, 28 Oct 2020 15:06:47 -0700 (PDT) Subject: Re: [XRF] How about Sodium? Randall, Wow that¡¯s going to be tough. #1 it has a Ka of only 1.04 keV with a 1 4% yield and # 2 its behind glass sucking up that 1.04. I can't say I've ever seen anything below Al and Al is tough in low concentrations. Down in that region you want a He or vacuum atmosphere and a detector set up for the low energies. It would be nice to see as Na Mg, K, Ca and Al will determine the basic mineralogy composition you're looking at. It is, however, fun to play with in water. Dud -----Original Message----- From: [email protected] [mailto:[email protected]] On Behalf Of Randall Buck Sent: Wednesday, October 28, 2020 2:27 PM To: XRF Subject: [XRF] How about Sodium? I asked before with no response but since you are now down at Ca, it seems appropriate to check again. Does anyone want a small sample of sodium metal, sealed under argon in glass. Sounds fancy but it is (they are) just low pressure sodium vapor lamps pulled from working fixtures. When cooled, the sodium vapor condenses to a small lump at the tip of the bulb (they normally run upside down). (I have the sockets and the 120VAC ballasts as well) Randall |
(X-Ray tube) edge-absorption type Source Filters De-Mystified
A nice tutorial link on the subject:
and another from Bruker, the XRF gun folks: essentially saying the same things, the first probably written by a tech the second by a sales person. From the first link this is what I needed to know, condensed down: To see an element, you must send in at least 2 keV more of energy to see that element. Source Filter: Allows you to focus on key elemental ranges to identify elements at detection limits The green filter is composed of 150 ¦Ìm (6mil) Cu, 25 ¦Ìm (1mil) Ti, and 300 ¦Ìm (12mil) Al. The green filter sees the optimization in a higher energy range, from 13 - 17 keV (Th, Rb, U, Sr, Y, Zr, Nb, Mo). Use 40kVp @30uA ? The red filter uses 25 ¦Ìm(1mil) Cu, 25 ¦Ìm (1mil) Ti, and 300 ¦Ìm (12mil) Al - with the red filter we end up with a zone of about 9 - 12 keV were there is an ideal signal to background ratio for elements (Pb, Hg As, Br, Au). Use 40kVp @30uA The black filter (250 ¦Ìm Cu/25 ¦Ìm Ti/300 ¦Ìm Al). You can see much higher peaks for the heaviest elements (Ba, La, ?Ce).?Use 40kVp @30uA or 45kVp @30ua for K¡¯s from La+Ce ? The above are the K-Edge type filters, utilizing the abrupt change in X-Ray absorption at the K (or L) edge of an element. Each element is different. These are effective and don/t require much in the area of exciter power. FYI what I'm doing with Cd and Al etc. metals is different and requires more power (or longer count times). The Cd for example is more of a secondary-target system with a built in attenuator. I like to think of it simply as a wavelength shifter. Both obviously work, in different ways. Geo |
Re: Cd Source Filter
Kovar alloy, 1 mil thick
Cd filter on source beam 40kVp @ 40uA Kovar is 54% Fe 17% Co 29% Ni Pic and .mca Try this on your non silicon, room temp? probe?? Thanks to member Wally C. for exotic alloys, long time ago. Geo Kovar-STAMP-300s-Cd-Beam_Filter.mca
Kovar-STAMP-300s-Cd-Beam_Filter.mca
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Cd-Beam-Filter-Kovar Fe-Co-Ni-Stamp1-notes-PUB.png
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Cd Source Filter
In earlier experiments (see Cd FAIL!) we gained information and data about how a cadmium (Cd) filter inserted into the exciter beam altered the output of that beam.
That allowed this experiment to use the altered output spectra for a specific purpose. A similar experiment has been on the back burner for a long time, specifically pointing the source, not at the intended target but an intermediate target, then using the rays excited from that target to excite the target to be analyzed. Up to 2 intermediate targets or crystals have been used in published experiments. Getting all that set up in my counting room would be impossible, due to the space required and the precision geometries needed. Not to mention my setup is not conducive for reflection geometries. Instead we investigated a transmission type filter (source filter) and learned form those experiments that a cadmium filter would seemingly pass through the Cd K lines at ~23 and ~26 pretty well, and block most everything else. The intention was to see if those monochromatic X-Rays would excited the intended target's K line XRF. It worked so well, I had to run the same test with the Ge removed to make sure I wasn't chasing a ghost. Both .mcas attached. Geo Ge-STAMP-20s-Cd-Beam_Filter.mca
Ge-STAMP-20s-Cd-Beam_Filter.mca
Ge-STAMP-20s-NO-Cd-Beam_Filter.mca
Ge-STAMP-20s-NO-Cd-Beam_Filter.mca
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Cd-Beam-Filter-Ge-Stamp1-raw-notes-PUB2.png
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Buddy can you spare 5?
5 seconds that is.
K-edge filter applied to bottom of wooden jig. Jig and pure tin sample placed in chamber Scanned for 5 seconds 50kVp @ 10 microAmperes.(the beam enters through shielded port in the bottom of the chamber) Sn_Si-PIN-5sec_50kVp-10uA_K-Edge-Filter.mca
Sn_Si-PIN-5sec_50kVp-10uA_K-Edge-Filter.mca
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Re: How about Sodium?
Randall,
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Wow that¡¯s going to be tough. #1 it has a Ka of only 1.04 keV with a 1 4% yield and # 2 its behind glass sucking up that 1.04. I can't say I've ever seen anything below Al and Al is tough in low concentrations. Down in that region you want a He or vacuum atmosphere and a detector set up for the low energies. It would be nice to see as Na Mg, K, Ca and Al will determine the basic mineralogy composition you're looking at. It is, however, fun to play with in water. Dud -----Original Message-----
From: [email protected] [mailto:[email protected]] On Behalf Of Randall Buck Sent: Wednesday, October 28, 2020 2:27 PM To: XRF Subject: [XRF] How about Sodium? I asked before with no response but since you are now down at Ca, it seems appropriate to check again. Does anyone want a small sample of sodium metal, sealed under argon in glass. Sounds fancy but it is (they are) just low pressure sodium vapor lamps pulled from working fixtures. When cooled, the sodium vapor condenses to a small lump at the tip of the bulb (they normally run upside down). (I have the sockets and the 120VAC ballasts as well) Randall |
Re: How about Sodium?
Thanks for the offer Randall, but Na.
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Geo ----- Original Message -----
From: "Randall Buck" <rbuck@...> To: "XRF" <[email protected]> Sent: Wednesday, October 28, 2020 4:27:26 PM Subject: [XRF] How about Sodium? I asked before with no response but since you are now down at Ca, it seems appropriate to check again. Does anyone want a small sample of sodium metal, sealed under argon in glass. Sounds fancy but it is (they are) just low pressure sodium vapor lamps pulled from working fixtures. When cooled, the sodium vapor condenses to a small lump at the tip of the bulb (they normally run upside down). (I have the sockets and the 120VAC ballasts as well) Randall |