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Recently I measured the sample: Si/SiO2(~300nm)/CuF2 (50 nm)/Au(~5nm).
I used INCA PentaFET -x3. It’s old but was serviced recently.
The information I want to extract is the Cu:F ratio. I noticed that when I use 10 kV I get a ratio of ~1:2, and for 5 kV, it’s ~1:1 (spectra were collected one after another on the same sample). I understand that with a higher acceleration voltage, I get deeper penetration. 10 kV beam reached the Si, while the 5 kV beam did not (Si : O ratio is ~1:2). But to me, it seems like the measurement done with 5 kV underestimates F (or overestimates Cu).
How does the software calculate the ratio?
What is the source of this difference?
📷
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Hello,
in EDS quantification is done under the assumption that the sample is (1) think, (2) flat, and (3) homogeneous.
This is not the case for layered systems, therefore the numbers are garbage.
An attempt to overcome this is using measurements with different energies. A free tool is BadgerFilm
​Reviews of EDS quantification (The vendors are usually reluctant in giving details of the calculations):
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Can we find main parental type of plastic by using values of EDX?
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No, the pure concentration of carbon in organic matter can not indicate plastic. As Stefania Koutsourea already stated in her first posting, you need other spectroscopies for that.
The items you show in you image are large enough to be analyzed e.g. by a confocal Raman microscope. Alternatively, there are also LDI mass spectrometric setups in which you can aim with a microscope.
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Hi,
I got an EDX measurement of relativly pure Aluminiumoxide impurities <0.05% so below the detection limit. I have a peak at 2 eV in addition to the expected energies. My guess is that it is a sum peak of photons from the Al at 1.5 and Oxigen at 0.5.
But how can I confirm my theory. And can someone explain to me when SUM peaks are happening and when they are not happening?
Thanks
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Thanks, very interesting review paper! Btw, it was finally published here:
And I hope the slightly... weird... English is now in better shape. But the content is definitely useful!
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Recently, we measured EDX/EDS of LaCrO3 crystals synthesized by hydrothermal method, and found that the characteristic energy for La and Cr are nearly the same for all of the noted energy levels. Could any one give some discussion on how the equiped software address this circumstance with a definite quantified analytic results?
Thank you in advance.
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Just to add a little explanation to Gerhard's and Warren's excellent answers:
If you have La, you will have La's L-alpha-1 and L-alpha-2 and L-beta-1 and L-beta-2 lines at about 4.6-4.7, 5.0, and 5.4 keV with well known intensity ratios. If you have La, you will have all of those lines.
If you have Cr, you will have its K-alpha-1 and K-alpha-2 and K-beta lines at about 5.4, 5.9 keV.
So if you have peaks at 4.6 but not 5.9 keV, you have all La and no Cr.
If you have peaks at 5.9 but not 4.6 keV, you have all Cr and no La.
If you have peaks at all of those energies, the software will compute the relative amounts based on the relative intensities of each of the emission lines (and other matrix etc factors).
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Hello everyone, I'm facing an issue with EDS software that prevents me from obtaining atomic or weight percentages for my scan. However, I do have access to the raw data, which shows intensity vs. energy with a few identifiable peaks. Could someone explain how I can use this plot to calculate the weight percentage of each element? I've already deconvoluted the peaks and identified the corresponding elements.
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I agree with Stefan Baunack, you should enlist the help of an experienced operator for these questions. I think we are serving that purpose on ResearchGate, but you should have a knowledgeable operator at your site. If not, you will find many results that don't make sense but which do have an explanation. Our service lab is setup with staff dedicated to the support of the instruments. Grad students do not have time to learn all the details.
I raise the question again about what the samples were coated with. I expect the peak around 2.1 keV is from a gold coating. It is very bad form not to label that peak.
The graph reminds me of why we did not choose EDAX for our system. Why are their major divisions at 1.3 keV? At least they are not using something even more inane like 1.34 keV. They really should use values like 2, 1, 0.5, 0.2 or 0.1 keV for major divisions. Minor divisions would also help.
The C level also reminds me why we chose Oxford. Even then, the C in this case is probably from contamination on the surface. It should probably be ignored. In the case of your PDMS, it must be dealt with.
I have attached some results for Fe and Cr standards on our system collected at various voltages. Neither have real C in the standard, but they were coated with 10+ nm of carbon. The C reports as ~5 wt% and 18 at%. But my C peaks look bigger than the C in the EDAX spectrum.
It would be nice to examine the correction factors that translated the intensity to mass fraction. While I cannot see the Phi-Rho-Z or ZAF factors directly, it appears that the composite factor must be over 2 in my case. It must be even higher for the EDAX case to come up with 21 wt%. As those factors increase from 1, they should be viewed with suspicion.
BTW, I would seriously doubt the V value. The V-Ka line falls right on top of the Ti-Kb line. It would be nice to see the fit both with and without V in the mix.
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I examined a compound containing lithium ions, and it did not appear in the EDX examination
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You are flirting with the truth but not quite there yet.
Li does produce x-rays. H and He do not having only electrons only in the first shell. It is unfortunate that the JEOL chart does explain that. The only reason that I can see they left it off is because the analysis is not practical. I see that my Oxford chart also does not show an x-ray line for Li, but their software shows the line at 0.054 keV.
One issue is the absorption of x-rays by the detector window. When I began working with EDS, Be was commonly used as a window. It effectively absorbed everything below Na. Thin windows became available and they allowed detection down to B, then down to Be as they were made thinner. I don't think they will ever get to Li with windowed detectors.
Now, Oxford and probably others have demonstrated the detection of Li using a windowless detector. The spectrum I saw was collected from a block of Li (100% before oxidation) and it showed a peak, perhaps weakly. That would not make for practical analysis.
Another issue is the strobe peak that is often present near 0 keV. On our Oxford system, that is centered around 0.015 keV. Under the shaping time that I use, that tails over across the Li position. At the highest resolution setting, it does not. But remember that because of the window, there is no intensity to be seen.
FWIW, I have recently been trying to analyze B in glass. Even that is near impractical. With 4% B, the precision is 0.4% for a 400-second acquisition. Be and Li would be worse.
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I want to know for doing EDX analysis to examine the elements present in the biomass, should I do the first pyrolysis or directly do the powder sample analysis? which one is the most favorable? please tell me.
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José Falcón-Hernández thank you sir for your response
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In my research, I have included a TEM image of grade 91 steel with point EDS. How to reply this question: "You still need to provide analytical TEM/EDX elemental mapping?"
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Thank you for your valuable suggestions @Kaushik Shandilya, and @Stefan Baunack.
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Analisei uma amostra sólida (em pó) em triplicata, para obter a composição elementar no EDX Shimadzu. O software me forneceu esse relatório (anexo) mas não estou sabendo interpretar.
Por exemplo: na parte quantitativa há elementos que não estão na parte qualitativa;
Na tabela quantitativa, o que são os demais valores além dos que estão em ppm?
Desde já, agradeço.
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I'll answer based on Google Translate, please ask again if it does not match what you actually wanted to know.
In EDX, you have to be careful about the background line which is substracted. The background covers a grand range of energies which will contain the range of elements not present and thus without a peak. Therefore, if you simply integrate the spectrum in locations of regular peaks, you will always get finite numbers, while if you subtract the baseline correctly, this will drop to zero.
Tl;dr: my main suspect is an improper baseline subtraction.
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Anyone explain the EDX Spectra and Elemental composition (at. % and Wt. %) of the dopant and composite. Why do we need both percentages?
No one explains clearly in the research article.
Everyone said, at.% and wt. % table given inside the EDX spectra. But, no one explains.
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Well, atomic (at) and weight (wt) percentages are different numbers and it makes a difference whether you are providing a stoichiometry or mass ratio.
Since these can be calculated from each other, providing one usually is sufficient, but it has to be provided what it is.
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The experimental values of atomic % and weight % are obtained by EDX spectroscopy.
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Hello, for atomic percent, the concept revolves around understanding the proportion of each type of atom relative to the total number of atoms in a compound. This is calculated by:
1. Counting the number of atoms of each element, which you usually derive from the compound's chemical formula.
2. Converting the number of atoms to moles, using Avogadro's number (approximately 6.022 x 10^23 atoms/mole), to relate the atomic scale to a more manageable macroscopic scale.
3. Calculating the atomic percent for each element using the formula:
Atomic % = (Number of moles of the element / Total number of moles of all elements) x 100
This calculation provides insight into the proportion of atoms in the sample that are of a specific element, a key understanding in the study of mixtures or alloys.
When it comes to weight percent, the focus shifts to how much mass each element contributes to the total mass of the compound. This is done by:
1. Determining the molar mass of each element (the mass of one mole of that element).
2. Calculating the mass of each element in the compound by multiplying the number of moles of that element by its molar mass.
3. Finding the weight percent using the formula:
Weight % = (Mass of the element / Total mass of the compound) x 100
This calculation is particularly useful in practical scenarios like preparing chemical solutions or manufacturing alloys, where the mass-based composition is crucial.
Both atomic percent and weight percent offer distinct yet complementary views of a compound's composition. Atomic percent relates to the quantity or 'number' of atoms, while weight percent pertains to the 'heft' or 'bulk' each element contributes. These theoretical calculations become even more valuable when compared with experimental data, such as that obtained from EDX spectroscopy. By contrasting theoretical values with experimental results, one can confirm the compound's composition or discover new insights, such as impurities or unexpected interactions within the material.
Well, this intricate relationship between theoretical calculations and experimental data is pivotal, propelling the fields of material science and chemistry forward and deepening our understanding of the substances that make up our world.
Regards
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How to calculate the Atomic and Weight percentage from EDX? Any formula to calculate the at.% and Wt. %?
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No sir. This is nota an answer to this question.
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I have obtained elemental percentages from EDX analysis, which include C, O, N, Fe, Al, Si, and Mg in varying proportions in my debris sample. I am interested in identifying the compounds present. Additionally, I have micrographs of the debris sample.
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Find a qualified EDS operator, and your task will be taken care of. Or describe your task in details and submit EDS raw results.
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Hi
Why it is important to have (gold) coating on your biological (plant) samples before EDX analysis? If the sample is thin, well attached onto carbon tape and I do not see any charging on sample, may I perform EDX measurement without coating? How coating infulence mesurements and how it influence final report (= weight percentage of individual element in sample)? I mostly use gold for coating
Thank you
Jan
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May be you'll find this useful:
Preparation of biological specimens for EDS with an SEM
​https://www.oxinst.com/blogs/preparation-of-biological-specimens-for-eds-with-an-sem
Tips and Tricks for Biological EDS
Advanced techniques in SEM and EDS for biological samples​https://www.selectscience.net/expert-insight/advanced-techniques-in-sem-and-eds-for-biological-samples/?artID=56957
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EDX provide weight % of elements present, while we need atomic wt % how to calculate?
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The atomic percentage is the number of atoms of that element, at that weight percentage, divided by the total number of atoms in the sample multiplied by 100.
So the atomic weight percent is calculated from the element weight percentage by dividing each element weight percentage by its atomic weight, do this for all elements in the sample, you will have a list of atomic proportions. Sum these together to obtain a total atomic weight. Then for each element in the sample divide its atomic proportion by the total and * 100.
Here is an example - using pyrite. EDX will give you
Fe: el wt% 46.55
S: el wt% 53.45
divide each by their atomic weights Fe (55.85) S (32.06) and sum
Fe: 46.55 / 55.85 = 0.833
S: 53.45 / 32.06 = 1.667
divide each by the sum (2.5) and turn into atomic percentage
Fe: 0.833 / 2.5 * 100 = 33 at wt%
S: 1.667 / 2.5 * 100 = 66 at wt%
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Kindly explain, how to calculate the elemental composition of weight and atomic percentage from EDX. Does anyone know the formula to calculate the at% and Wt%?
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P=basınç, Ma =molekül kütlesi, %=doğada bulunma oranı, d =özkütle, R =sabit, T =sıcaklık
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Please see the attached pdf for the EDX scanning results. I would like to know whether the nanofiber in the SEM image contain silver.
Thank you.
BRs,
David
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I first thought that Vladimir's janitor comment was a little harsh, but then I looked at the results more closely.
Why aren't the C, O, and Au peaks labeled? They are significant features in the spectrum, but they are not quantified. I understand that Oxford (and others) will factor out the element from the coating, but it is very risky to ignore C and O when they are clearly present, even if they are from a carbon tab.
There are no clear peaks for F, Na, Al, Si, or Ag, but those elements are all quantified with some rather ridiculous results. The sigma values indicate that values are not to be trusted. Frankly, I think the values should have been higher. I cannot believe the F value is 80% with only 13% sigma.
I would like to see the fitted spectrum. I suspect that F is being used to account for the O peak since the O was not measured. Oxford would let them deconvolute the O peak then ignore it, at least in the full version of the software (not in Aztec One). I would also like to see the report of the net peak intensities so see if the numbers are reasonable.
Consider that the Au peak is probably from 10 nm of gold, but the signals from F, Na, Al, Si, and Ag are all MUCH less than the Au peak.
What is the fiber supposed to be made of? The image looks like SE. Was anything recorded in BSE. Is there reason to expect the heavier elements. From this evidence, I suppose the fiber is organic.
Were these spectra definitely from the fiber? Could the image have drifted? We have Oxford's AutoLock feature for tracking features in cases of image drift. Even then, we sometimes fail to track features and we end up with spectra from the surroundings. It would have been nice here if the operator collected spectra on and off the feature to see if there is any difference. They might also have scanned across the fiber, as you suggested.
Finally, lower voltage would have been better. I usually run at 10 kV for starters but might have tried 6 kV in this case. And include a BSE image.
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Why are other elements such as calcium, oxygen, sodium, magnesium, aluminum, silicon and molybdenum visible in the EDX spectrum of tapered optical fiber (SMF‐28) covered with palladium and copper by sputtering method? Do all these foreign elements like silicon belong to the optical fiber itself?
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Dear Prof. Korea,
Thank you so much for your nice response. Your detailed response helps me a lot. That was great.
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I did EDX for my nanoparticle samples. It contain peak for Cl, C, Na, O and Ag . What is the meaning of this peaks. Where does the other elements come from? Kindly provide the interpretation reference files.
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The information you provided is insufficient to understand which elements are desirable and which are not. As can be interpreted, you have Ag nanoparticles. But are they functionalized or modified? Have they been dispersed in a solvent and then dried completely before analysis?
As mentioned by others, C and O are pretty common to appear during EDX measurements. You need to know how much is the elemental composition to say if it is coming from your material or not.
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I am looking for where I can carry out the following instrumentation analyses.
SEM with EDX (5um, 10um and 20um) for powdered samples
SEM with EDX (5um, 10um and 20um) for polished surface samples
XRD (Rietveld Mineralogical analyses) for powdered samples
Any credible suggestions or recommendations?
Thanks
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Sage. Davies Pearl Oluwatosin - Allschoolabs Yes, I made enquiries, and I was told Allschoolabs doesn't have up to 5um, 10um and 20um magnifications for SEM.
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Its about synthesized materials characterizations
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please have a look at the following test facility in Lahore:
Best regards
G.M.
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How the EDX results significant with the stoichiometry? Please anyone explain this and provide the appropriate references?
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EDX results contain usually weight percentage and atom percentage of the elements present in the sample. By analyzing the atom %, we can understand the compound/phase. For eg., if EDS analysis give approx. 66%Al and 33%Cu, then the phase is possibly CuAl2. We can also convert to eqvt wt% for verification.
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Given wt% of Ru, Ti and O. Can we calculate wt% of RuO2 and TiO2 from the given EDX data?
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you may 'google' for that stuff...
It is simple calculation dealing with atomic and molecular weights...
One of the results may be for example the following tutorial:
Please go through it and apply the procedure to your sample system...
Good luck and
best regards
G.M.
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Hello everyone,
I have a soil sample in which soil organic matter was stained. To find out how effective and specific the staining was, I want to map the spatial distribution of both organic matter and the staining agent. The idea is to do that with EDX measurements on a thin section of that sample.
The problem is that epoxy resin, which is typically used as the embedding material, is an organic substance itself. So, is there a possibility to differentiate between resin and soil organic matter using EDX measurements? Or would it be possible with any other chemical surface analysis? (I have never done any of these, so please talk like to a beginner on that area.)
As one idea, I read about adding a dye to the resin that is visible under UV light (doi:10.1016/j.geoderma.2012.02.023). Maybe something analogous is possible for EDX measurements?
Another idea, can one distinguish between them based on functional groups? Is EDX capable of measuring that?
Are there embedding substances that would be easily distinguishable from soil organic matter?
I am pretty sure someone has had this problem before, so I hope the solution is out there, too. Thanks in advance to the one(s) reporting it here.
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Rana Hamza Shakil
, J. C. Tarafdar ,
thank you both very much for your well thought out answers! I apologize for answering so late, other activities kept me busy and now I return to the topic. So again, thank you very much!
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How can we prepare our electrode to use SEM , DRX,EDX, FTIR,XPS and CV characterization?
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Your question is very unspecific.
First, you should read papers about your system.
1) In the experimental section of the papers the preparation should be (at least shortly) mentioned. For special samples one might dig out underlying PhD thesis, were often more details are mentioned.
2) In textbooks about the specific method preparation should be mentioned.
3) I guess you will not do all the analysis with the different methods yourself: discuss it with the operators: which methods are already available and tested.
4) The methods you plan to use may require different preparation, e.g. several samples.
5) What is DRX?
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We can use EDX to measure the silver concentration before and after leaching test to know amount of silver leached. However, the concentration of leached silver from membrane is measured using ug/L or mg/L with the aid of ICP-MS. How to measure the silver concentration before leaching test of membrane using ug/L or mg/L unit?
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X-ray photoelectron spectroscopy (XPS) is a surface chemical analysis technique that can be used in the elemental analysis of silver.
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EDX can detect C O but why its not detecting N H
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Hydrogen has no characteristic X-ray emission
Nitrogen can be detected using EDX, but there are two problems:
1.low energy x-rays are strongly absorbed by the sample
2. characteristic X-ray radiation also occurs with the participation of valence electrons participating in the chemical bonds of the element - thus, the shape and position of the peaks may differ in different compounds. Standard samples must be used for accurate measurements.
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I am trying to calculate the percentage of retained austenite in Maraging steel through XRD analysis.
How can the chemical compositional % of each element present in the martensite and retained austenite be calculated in order to determine the amount of retained austenite using XRD? In addition, which one contains more iron (Fe): martensite or retained austenite?
ICP provides data for the entire alloy and not for the individual elemental composition of each phase. Can we utilize the EDX results to determine the composition of each individual phase, though?
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Dear friend Qanita Tayyaba
Determining the chemical composition of individual phases, such as martensite and retained austenite, in a material like Maraging steel requires advanced characterization techniques. While XRD analysis can provide information about phase identification and phase fractions, it does not directly provide information about the chemical composition of each phase. However, there are complementary techniques that can be used to determine the elemental composition of individual phases.
One commonly used technique is Energy-Dispersive X-ray Spectroscopy (EDS or EDX), which is typically coupled with scanning electron microscopy (SEM). EDX analysis can provide qualitative and quantitative elemental composition information within specific regions of interest. By analyzing different areas of martensite and retained austenite using EDX, it is possible to determine the elemental composition of each phase.
To calculate the percentage of retained austenite in Maraging steel, XRD analysis can be used to measure the phase fractions. However, to determine the chemical composition of each phase, EDX analysis or other techniques like electron probe microanalysis (EPMA) or wavelength-dispersive X-ray spectroscopy (WDS) would be more suitable.
Regarding the question of which phase, martensite or retained austenite, contains more iron (Fe), it depends on the specific alloy composition and heat treatment conditions. Generally, martensite is a solid solution of carbon and iron and contains a higher percentage of iron compared to retained austenite, which is a metastable form of austenite. However, the exact iron content in each phase can vary based on the alloy composition and processing parameters.
For more detailed information on determining the chemical composition of different phases and the iron content in martensite and retained austenite, I recommend consulting the following references:
1. Bhadeshia, H. K. D. H. (2017). Martensite and Bainite in Steels: Transformation Mechanisms, Mechanical Properties and Applications. Woodhead Publishing.
2. Ceschini, L., Bartolucci, G., & Rambaldi, E. (2010). Characterization of retained austenite in maraging steel: Comparison between different techniques. Materials Science and Engineering: A, 527(4-5), 1198-1206.
3. Li, L., Li, W., & Huang, M. (2019). Quantitative analysis of retained austenite by X-ray diffraction. Materials Characterization, 147, 61-70.
These references provide insights into the analysis of retained austenite and the determination of elemental composition in different phases of steel alloys.
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I am a university student and I've been doing EDX analysis on some kanthal heating wires and one of them appears to have a huge amount of carbon in it (one reading said 20% the other said 25%), which is very unexpected and I cannot explain it (in the report I'm writing that's due tomorrow, and I don't have time to repeat the EDX analysis), apart from as contamination from a fingerprint (as I was a bit clumsy while preparing the sample for the SEM), does anyone with experience of EDX think contamination could leave such a high amount of carbon on the sample?
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Typically, fingerprints contain other elements, like electrolytes, in addition to C. If I'm trying to determine if something might be a fingerprint, I also look for low levels of O, Na, and Cl. May also see K and S.
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Dear researchers, in my EDX spectra there is peak of Al and Mo though I don't use any material related these elements peaks in my sample, I think it will be impurity peaks. but I performed the experiment very hygienically.
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I have encountered lines of elements that were definitely not part of the samples when the surface of the sample was uneven. If it is inclined to the plane of the holder or if there is a strong roughness.
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Some of the results of EDX analysis are quite scattered e.g. for Ca K: from about 3% to 27% at. They agree don't with the atomic composition of the compound. Any comment on it? Please answer
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Dear Yaseen Muhammad , you may share your EDX spectra;
there might be a superposition of Ca K-radiation with the L radiation of for example of
Ca K-alpha (~3,69keV) <--> Sb L-alpha ( ~3,6 keV )
or
Ca K-alpha (~3,69keV) <--> Te L-alpha ( ~3,77 keV )
In order to avoid such superposition you should go for an excitation energy of just above Ca K-excitation (e.g. 4,1keV; Ca K-edge ~ 4,04keV).
The L-edge/binding energies for Sb and Te are above that energy value and their L lines should not show up at all in this case.
Best regards
G.M.
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The peaks in EDS appears less then 20Kev
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the excitation energy of the electrons has to be larger than the x-ray photon energies energies of the equivatent x-ray emission lines, which in your case are below 20keV.
For example for Ag (Z=47) the Ag K-alpha ( ~22keV) and Ag K-beta line ( ~24,9keV) you have to excite the Ag K-shell electron having a binding energy of about 25,5 keV. Thus in this case the electron energy has to be larger than 25,5 keV.
For elements of atomic number Z being smaller than that of Ag (ZAg=47), you may also use that electron energy.
For the emission lines and excitation energies (edge energy) of the elements please have a look for example at the 'x-ray data booklet'...
Best regards
G.M.
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Quantification of EDX spectra of Al-based casting alloys it was found certain intensity of Zr (up to 0.7 wt. percent) whereas the chemical analysis showed only very little Zr content (0.05). EDX were performed using Talos 120 TEM. Any Zr-enriched precipitates were not observed. I am looking for an answer why Zr intercity appeared in the aluminium matrix whereas it can't be. Many thanks in advance
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Dear Mykhalenkov, I will be performing the TEM analysis of as-cast Al alloys soon and will let you know if I encounter this problem.
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EDX show inadequate result: Mn 4.8% Fe 38.9% O 55.4%. that is not connecting with our formula of compound. Can EDX mix up the spectrums of Mn and Fe or it is a mistake from the synthesis?
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No
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Hi all,
I have a sample of ZSM-5, and i don't know the ratio of Si/Al. I want to calculate the ratio with the result of EDX/SEM. could you help me?
Bests,
Samira
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With EDX you can collect the spectrum of your sample and obtain a table with the amount of the elements expressed in weight percent and atomic percent. So it is simple to calculate the ratio beteween some of them
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How we can interpret the presence of Hf peak in EDX spectra of reference birch wood ? While I have not seen this peak before in wood samples.
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thank you dear Jürgen Weippert . in fact, I have a silica coated wood spect that is good. but on control wood samples there is this Hf peak. there are usually variety of inorganic martials in wood as a sediments in too low amount(less that 0.5 %). but this peak is not normal in related literature
please see attaches file.
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It was not possible to identify lithium an nitrogen. What is the effect of the Be window in this case? Can this be explained with the K-Shell of nitrogen?
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The nitorgen peak should appear between the C and O peaks. I wonder if the substrate x-rays are affecting this area of the spectra.
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Is an EDX analysis of lithium nitrate possible? I have not been able to identify lithium nitrate. Are there any possible explanations for this? If possible, also cite literature sources.
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If you system can identify C and O, that means that your specimen has no identifiable quantities of N.
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My substrate is Magnesium, it was electroless "Ni-P" coated.
I went to another test facility for EDX test to verify the contents of the coating. A Pt coating was put on it prior to FESEM and EDX at the test centre. As a result, the EDX pattern showed Pt peaks when the findings were released. But only Nickel and Phosphorous were deposited on the substrate in my work.
SO should I just ignore the Pt content in the EDX results or not ?
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Thank you Gerhard Martens . Yes , I'm having the same issue you mentioned. The peaks for P and Pt are close together, and the wt% for Pt is 6 vs to P's 3 and Ni's remaining. How will I portray the EDX data if I omit the Pt wt%? How accurate and reliable will the new composition be?
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Recently, I have deposited the LiF on silver foil and I have done both XPS and TEM/EDX of my sample. EDX shows no oxygen presence or any other impurity in the LiF sample. SO, Is it possible that oxygen we got from XPS measurement, does not segregate in grain boundary or phase boundary?
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EDS+TEM is pretty difficult technique to implement properly. For example, operator could choose too short dwelling time, and then nothing but main compnents would be found. By the way, how thick are your LiF layer and silver foil?
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How many frames are needed to cover 1cm2 area with a 50-micron step?
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Alexander Bolshakov Why not ask the manufacturer?
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Energy Dispersive X-Ray Diffraction (EDX)
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What is the difference between EDX and EDS for caracterisation of nanoparticles.
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EDX: refers to the method or EDX analysis.
EDS: refers to the equipment; Energy Dispersive Spectrometer.
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Hello,
I am looking for traces of PTFE in the nickel plating on a steel sample. I have no prior experience with SEM technology. I have access to a JSM-IT100 SEM. Based on my research, it appears possible to determine the amount of PTFE present utilizing the machines EDS/EDX system? However I do not know how to go about this problem. Any help or direction is much appreciated.
Thanks
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Too little information to give really useful advice.
If you are looking for islands of PTFE on Ni, then simple SEM observation could help (in secondary and backscattered electrons). EDS should be used to check whether F is present in islands. For "quantification" you can determine relative area of islands.
Anyway, you can start with observation and checking if F present in different areas of you specimen. May be you'll need to make cross sections of your plating.
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I have two powder materials in particle size about 30 Micro-meter, one consist of CuO and TiO2, and other of CuO and MgO. I received following results from EDS operator. My questions are:
1-Did you think the test penetrated the sample completely?
2- If so, how can I get the result on the surface for my case or what is minimum energy required for my elements ?
3- What are these red and green vertical lines?
4-In general, how can we interpret EDS spectrum?
Note: regarding carbon that appear in result the operator said me that its due to he used material consist of carbon to fix the sample in the device is this acceptable for publication or how can I deal with it ?
Thank in advance ,,
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the penetration depth of the exciting electrons is in the very low µm regime, even below 1µm, and is depending on the acceleration voltage. The penetration depth/ attenuation length of the x-ray fluorescence is also the low µm regime.
Thus, with respect to your 30µm particles, you will not 'see' the core of them.
Unfortunately, low µm regime is not surface or surface near region. Here you have to go the photo electron spectroscopy, as it has been suggested by Jürgen Weippert .
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Hello,
I found a specail clay mineral in shale sample.
Backscattered SEM image and corresponding EDX spetrum of a argon-ion milled shale sample were attached. The caly mineral looks like rose-like authigenitc smectite in the SEM image. But since element k is present, it could be illite. It also could be a mixed-layer illite-smectite (I/S). Can anyone tell me what is the kind of the clay mineral?
Thanks for your help.
Chuanmin
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Without analyzing by XRD technique the parallelly oriented clay samples saturated with Ca and K ions and subsequent glycolation of Ca-sample and heating the K-sample , it not possible which clay mineral it is.
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Element Atomic% Wt%
O 50.2 19.79
Zn 49.8 80.21
Total 100 100
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Dear Zyoud
From my point of view, EDX is useful just to perform simple and rough elementar chemical analysis. As mentioend before, the % of error is a critical drawback. I reccomend you to search for XPS analysis. Then, you have a characterization technique that will provide elementar composition, molecular information (oxides, nitrides, etc) with a suitable precision for quantification.
Have a good work !!!!!
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We are looking to characterize "fluorine flowers" on the surface of aluminum pads. Essentially characterizing contaminates present only on the surface of a homogenous material. So the poor surface sensitivity of EDX is a major limiting factor for us. This would be more of a monitoring effort, so getting relative values in comparison to a golden sample would be fine. Would you all have any techniques that might help, or papers that have addressed similar issues?
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You may want to try low voltage operations (as was suggested by Adeyinka Aina ). I would choose 3 kV, good enough to excite both F and Al.
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I already did TEM/EDX analysis. The results show K factor value, wt% and Atomic%.
How I convert the results by calibrating with ZAF standard.
Example:
Element K factor wt% Atomic%
O 1.455 8.83 14.53
Si 1.000 91.17 85.47
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Dear Muhammad Aleem Zahid , your question is a bit fuzzy. I believe you made standardless "quantitative" TEM/EDS analysis of Si-O compound and you are not happy with results. You cannot "convert" data you already have. By the way quantification of specimens like yours with TEM/EDS is nearly impossible. Of course if you have suitable (certified?) SiO2 foil to serve as a standard, you may want to try.
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How deep can the x-ray penetrate through aluminum nitride (AlN) sample with an accelerating voltage of 10kV (EDX model : FEI Nova NanoSEM 450 SEM)?
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To have an idea of the penetration depth in your sample you can use the classical formula of Kanaya Okayama (you can search it on google)
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I have gone through some threads, and I found, for example, an x-ray attenuation length calculator (https://henke.lbl.gov/optical_constants/atten2.html); it seems simple, but I did not know the parameters such as "Scan" what should I insert here. My questions are: is this reliable way, and how can I use it? Is there any other way or software?
Best wishes
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thanks for feedback.
You are right; theta is the angle between the incoming primary x-ray beam impinging onto the XRD sample.The angle between the sample and the diffracted x-ray beam leaving the sample and entering the detector also has the value of theta. So the beam geometry of the XRD set up is just a symmetric reflection set up.
I am sure, you are aware of that issue.
This theta is also the parameter of the x-axis of the XRD pattern, but unfortunately displayed as x=2*theta*) due to historical reasons.
You are right; the penetration depth is not constant for the whole XRD pattern, but varies along the x-axis according to the equation given above.
So the x-ray penetration depth for the 'peaks' (at specific 2*theta positions) is alo different according to that equation.
*) 2*theta is the total deflection angle or scatter angle of the primary beam
Additional remark:
the penetration depth (or better 'information depth') for EDX, as you have asked in your question above, is more complicated due to two facts:
a) different angles with respect to the sample surface (e.g. thetap for the primary exciting beam and thetad for the detected beam) and
b) different linear attenuation coefficients for the excitation radiations (e.g. named as µe(Eex)) and the x-ray fluorescence ( e.g. named as µf(Efl)). Both attenuation coefficient depend on the photon energies, which are in use, such as the (mean) excitation energy Eex and the fluorescence energy Efl of the detected x-rays
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how can we analyze EDX data?
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Your query is similar to the attached link. Please find out. It might be helpful to you.
Best regards
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I think it is of material API X-65
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Similar to Alexey Fedorov , I recommend not concluding anything from this image. This is not sufficiently resolved, maybe try AFM if your SEM can't get it better?
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Can I detect a thin layer (a few dozen nanometers) of SiO2 on surface of silicon carbide wafer by EDX?
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SEM and EDX cannot be used for nanometer-thick layers. You need at least 100 nm, but reliable results are possible from 1-2 µm.
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What are the possible characterization techniques to confirm the formation of a core-shell nanostructure except for TEM? How can we confirm it using EDX technique?
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Core shell structure can be confirmed by stereo microscope technique
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Hello, can anyone help me with interprétation of the quantity of lead in this sample
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You need to repeat your analysis. There are lines on your spectrum (possible O and Si) that were not taken in account. It looks like Pb alaysis was performed on M lines, which are overlapping with Si line. You need use L lines, but then it's better to repeat X-ray acquisition at 20 kV. Without using L lines it's mostly impossible to say if presence of S is real and not an artefact produced by software. And if you were using standardless analysis (and I am sure you were), then results for C (and O) are mostly useless.
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I want to know that TBO is used for the quantification of heparin on the PCL, Why?
Why can we not used FTIR or EDX?
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You may wish to look up the work of ML Wolfrom and JR Vercellotti. Also see doi: 10.1002/9780470110447.ch4.. 1977;24:203-312.Methods Biochem Anal
Determination of heparin and related sulfated mucopolysaccharides by L B Jaques
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I am using 2M NaOH solution for synthesis of zinc oxide nanoparticles, my EDX data is showing presence of Na and OH. How can I remove it completely? As I am washing it 6-10 times with distilled water and ethanol...but still there is presence of NaOH. Can anyone suggest how can I remove it?
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Dear Puja,
many thanks for sharing this very interesting technical question with the RG community. iI fully agree with Alan F Rawle and Alec Ladonis in that key points here are thorough washing of the initially obtained nanoparticles with distilled water (even more often than 6-10 times) and exclusion of moisture from the calcinated end-product .
This leads me to a question I would like to ask all experts in this forum: Is it possible to make ZnO nanoparticles without any annealing / calcination step? In this context please have a look at the two papers cited below in which this has been reported. As you may know, I'm a synthetic organometallic chemist and not a nanoparticle guru. However, to the best of my knowledge these low-temperature routes will only produce Zn(OH)2, but no ZnO. Please let me know if I'm wright or wrong in this point.
Here are the two articles:
Preparation of ZnO Nanoparticles without Any Annealing and Ripening Treatment
and
A Quick Process for Synthesis of ZnO Nanoparticles with the Aid of Microwave Irradiation
Both papers are freely avvailable as public full texts on RG.
With best wishes, Frank Edelmann
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Other elements include Ca, C. All elements are given in wt %.
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Although EDX microanalysis provides some information, it is always better and safer to combine more methods. The corrosion product can be analyzed, for example, by powder X-ray diffraction analysis. Corrosion products are usually mixtures and may contain an admixture of precipitates such as gypsum and calcite or aragonite.
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Please help me understand the attached EDX spectra.
I'm not really familiar with this analytical technique and it is my first time to use EDX.
What is the difference between Element Wt% and Atom %?
And can EDX detect noble gases?
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The weight percentage of an element is the weight of that element measured in the sample divided by the weight of all elements in the sample multiplied by 100.
The atomic percentage is the number of atoms of that element, at that weight percentage, divided by the total number of atoms in the sample multiplied by 100.
So the atomic weight percent is calculated from the element weight percentage by dividing each element weight percentage by its atomic weight, do this for all elements in the sample, you will have a list of atomic proportions. Sum these together to obtain a total atomic weight.  Then for each element in the sample divide its atomic proportion by the total and * 100.
Here is an example - using pyrite. EDX will give you
Fe: el wt% 46.55
S: el wt% 53.45
divide each by their atomic weights Fe (55.85) S (32.06) and sum
Fe: 46.55 / 55.85 = 0.833
S: 53.45 / 32.06 = 1.667
divide each by the sum (2.5) and turn into atomic percentage
Fe: 0.833 / 2.5 * 100 = 33 at wt%
S: 1.667 / 2.5 * 100 = 66 at wt%
so twice as much by the number of atoms of S as Fe, FeS2, but similar-ish wt% because Fe atom is much heavier than S atom.
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EDX - energy dispersive x ray
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Interesante pregunta, espero las respuestas aportadas por los expertos cumpla sus expectativas como investigadora.
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Dear expert colleagues, it is a well-known fact that SEM-EDX analyses give acceptable results from about Na on (i.e. no precision is expected for light elements as O, C, N, and so on). My questions are the following:
1. Let us assume that we have EDX atomic% data on a surface, containing C, O, and heavier elements. If the data on O and C are not precise, can we still trust the relative atomic % values of the heavier elements? Or we should treat the whole thing semiquantitatively? What about changes and tendencies? Are they reliable?
2. If we use wavelength dispersive analysis, do the atomic% values become reliable and comparable with those of the heavier elements?
3. How do EDX and WDX compositional data compare with XPS or XRF atomic% data? Can EDX and WDX data be used at all without model-matrix studies?
I would appreciate it if you could quote review articles on these aspects. So far I have tried to find some, but I did not find what I really looked for. It would be helpful to hear the opinion of colleagues who use these methods in their daily practice not only for elemental mapping but also for obtaining (semi)quantitative compositional data.
Thank you in advance
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First of all, having a light element matrix might not be detrimental to quantitative EDX (or WDX) : it all depends -as Vladimir Dusevich said- on having a "good" SEM (well calibrated for quanti), being a "good" operator (knowing what to do and more importantly, what NOT to do), and having "good" standards" (or having proved that one of the quant models works on your samples/matrix).
It is easier for example to quantify heavier elements in a light matrix that is suited for quanti, than for instance Carbon in Steel (for which EPMA would be used).
One of the ground rules would be : if your sample is not smooth, dense (non porous), homogeneous, conductive, isotropic and finally thick enough for electrons not to strike through ; then you can probably forget about precise quantitation by SEM-EDS (or WDS, does not matter).
Plus, you should be aware that "standardless" analysis, (whatever the model, ZAF, PhiRhoZ, P&P...) as provided by all manufacturers is always worse than having your personal standards, ideally on the same matrix as that you will be analyzing (most always difficult to do).
If you're not familiar with quant SEM-EDS, you might want to start with : https://www.springer.com/gp/book/9781493966745
D.E.Newbury again...
I could suggest French books as well if you read French (lots of work done in France on quant SEM-EDS models back in the 70s and 80s).
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Most of the journal articles show that the plasmon peak of silver nanoparticles exists at the wavelength range of 400-500 nm. However, what I get is at around 550 nm (the AgNPs were synthesized through chemical reduction of silver nitrate by sodium borohydride with the presence of dodecylamine as capping agent). The formation of AgNPs has been confirmed by other elemental analysis (XRD,EDX). So I am not sure that does the peak presences at the wavelength of 550 nm is attributed to AgNPs or not?
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Dear all, if NP's aggregation and/or the dielectric environment are behind such shift, it is good to have a look at the following document. My Regards
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Hello,
I have the data/results from XRD and EDX. The EDX data shows chemical %age, e.g. SiO2: 73.653 % , Al2O3:14.426 % and other etc including some other details. The XRD results include, peak data Chart (2θ vs I unit cps); 2θ, d and counts table and peak %ages etc.
what is the procedure to calculate the minerals %age, specifically, quartz and montmorillonite and other minerals. Please try to have a simple and concise answer/procedure. If you have a flow chart or outlined procedure or an example data, would be much helpful.
Thank you.
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Dear Mazhar, many thanks for asking this very interesting technical question. In this context please have a look at the following relevant link which might help you in your analysis:
Use of TEM-EDX for structural formula identification of clay minerals: a case study of Di Linh bentonite, Vietnam
This paper has been published Open Access and is freely available as pdf file (see attached).
Good luck with your work!
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Using Si substrate as base material for ITO samples, after EDX analysis ,not only the samples compositions or content increased or decreased, the Si (as base material) content as well also increased, why?
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some ideas:
a) I do not know your ITO layer thickness,
but when during annealing for example oxygen goes off the sample the exciting electrons may more efficiently strike the substrate and thus will increase the excitation of the Si fluorescence.
b) When the annealing will induce cracks in your ITO layer then your Si substrate is partly open for direct electron bombardment and Si fluorescence will show up.
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Dear colleagues,
I am a researcher working with bovine hydroxyapatite. I want to reduce the percentage of carbonate on the sample. Is there any suggested techniques for this? I am measured the carbonate from EDX (SEM-EDX). Thank you
Thank you.
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Dear Maria Apriliani Gani,
These may be addition of impurities, high temperature and environmental conditions can reduce the formation of carbonates.
Bone mineral is not pure hydroxyapatite. The small, plate-shaped (20–50 nm long, 15 nm wide, and 2–5 nm thick) apatite crystals contain impurities, most notably carbonate in place of the phosphate groups. The concentration of carbonate (4–6%) makes bone mineral similar to a carbonate apatite known as dahllite. Other substitutions are potassium, magnesium, strontium, and sodium in place of the calcium ions, and chloride and fluoride in place of the hydroxyl groups.These impurities can reduce the crystallinity of the apatite , and, in doing so, may alter certain properties such as solubility. The solubility of bone mineral is critical for mineral homeostasis and bone adaptation.
Carbonate substitution in apatite each control the crystal’s perfection and crystallite domain size, affecting material properties, in different environmental conditions. High temperature substitution methods indicating a higher energy barrier for the formation of carbonate.
Ashish
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i. Scanning electron microscope (SEM) coupled with energy dispersive X-ray (EDX).
ii. X-ray photoelectron spectroscopy (XPS).
iii. X-ray diffractometer (XRD).
iv. Fourier transform infrared (FTIR)
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Is the signal too noisy? Energy too low? Are all TEM EDX detectors above the sample? There are detectors of electrons below but no EDX. I just wonder why this is.
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in addtion to what Gerhard Martens has already mentioned, I think that you'll get a much higher background due to Bremsstrahlung radiation in foreward direction. So smaller peaks are added on a larger background ... Best regards, Dirk
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We're trying to get to the stoichiometry of bacterial cells through EDX combined with SEM or TEM. Which kind of grids do you think is the best for our sediment freshwater bacterial cells?
Thank you very much!
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Bacterial cells are not stoichiometric. So, I believe you want to know cells composition. EDX is not the best (may be one of the worst) methods to quantify composition of a biological matter. If you are interested in a relative quantities of some heavier element, you can use any grid but the grid containing element of interest. If you want to get "cleaner" spectra (with no stray radiation from a grid) you can use Be grids. For SEM you can use carbon substrate.
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I've synthesized 45S5 bioglass by sol-gel method and my XRD and FTIR results are similar to 45S5 bioglass but my EDX result has differences and instead of Si and Na the amount of Ca is higher. Could you please tell me what is wrong with that?
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Hi Negar,
I'm not sure whether you have collected multiple EDX spectra or just one spectrum. If you collected just one spectrum and saw a significant difference in Ca content compared to other spectroscopic analysis, this could be due to a local aggregation of Calcium in that particular area of the sample. Keep in mind in EDX, with high magnification, the spectrum is collected from a very small area of the sample. Therefore you might want to collect multiple spectra from different locations of the samples before making general conclusions about the sample. Also, EDX is a surface analytical technique. Therefore the surface elemental composition you get from XRD has a possibility to differ from the other spectroscopic methods if you crush / powder the samples for the analysis.
I hope this helps and good luck with your study!
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I have electrodeposited Co, Ni and Cu oxide on FTO glass substrate from equimolar conc. bath and EDX data obtained is attached here. Kindly guide how can I calculate the composition of my oxides?
Note: XPS confirmed +2 oxidation state of metals.
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First, you have to move from WT% to AT%. To do that, you have to divide each element WT% value by the corresponding atomic mass, so you get the number of atoms of that kind contained in 100 units of total mass. Then you must sum up all the numbers obtained, to get the total equivalent atoms number in your base 100 unit mass of material. By dividing each number obtained in step 1 by the above said total equivalent number, you get an estimation of the AT% of each component in the probed material.
For example (taken from your table), the WT% of Oxygen you probed is 22.84% (22.84 mass units over 100 mass units). The O atomic mass is 16. You divide 22.84 / 16 to get 1.42, the O equivalent atoms number. Doing the same for all other components you get the Sn, Cu etc equivalent atoms number. Than all such number will sum up to 2.39 (approx). The AT% for Oxygen will be 1.42 / 2.39 = 59.4%.
After you got all the AT% values, you may have a rough idea of the coarse stoichiometry of the oxides (it is clear from your table that a large part will be SnO2 from the FTO substrate).
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I am wondering why there is a variation in the theoretical atomic percentage in Ni-Cu ferrites and the percentage atom values found from EDX spectra. In the case of Fe and O, there exists this difference for all of my samples. If it exists the same after the second or third trial from EDX spectra, how can I explain the reason for this discrepancy in the literature? Would you please provide your explanation with references? As I saw from the literature, people usually do not talk about the difference in calculated and observed values of atomic percentage, rather they find whether all elements are present in the spectra and the total should give 100 % atom.
Thank you in advance.
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Quantitative EDX analysis for your specimens is very difficult task because of presence of oxygen. You need highly qualified operator and set of rather expensive standards. If you really need good analysis go for some other method, not EDX. If your specimens do not differ in composition too much, you can compare heights of peaks: higher peak, higher concentration. By the way EDS and EDX are interchangeable abbreviations, EDX being a bit more precise in meaning, and EDS being used a bit more often.
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I have taken EDX of a ceramic compound and It has shown all the expected elements along with different weight and atom percentage. But in XRD data of the same compound, all the elements have not been observed in a crystal. How I can sure which compound is developed?
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There is not a specific relation between XRD and EDS patterns, because XRD detects the crystalline phases, but EDS shows only the elements. I mean EDS is a chemical analysis but XRD is a phase analysis. In general, EDS cannot detect light elements such as B or C precisely. Meanwhile, low content phases may not be detectable by XRD when their percentage is less than 8. Additionally, you are only able to identify the crystalline phases (compounds or elements) by XRD test. I mean, if a phase is in its amorphous state, it cannot be detected by XRD, whereas its chemical composition is easily detectable by EDS.
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I fabricated a composite say AB and both are carbides ceramics having formula AC and BC. I did EDX point analysis and observed A (45 wt %) and B (28 wt %), Carbon (26 wt %) and Oxygen (1 wt %). Can this data confirms the formation of A rich (A, B) C solid solution? Also at one location I got Carbon (83 wt % ), Oxygen (16 wt %), A (1.62 %) and B (0.13 %). Does that means precipitation of carbon at grain boundaries ? In EDS elemental mapping for some composition both element A and B mapping are superimposing at most of the places. Does it means formation of a intermetallic compound AB or it may be (A, B) C solid solution ?
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In addition to EDS you need to study microstructure to see if you really have a single phase specimen. BSE imaging and/or etching should help, If you want to quantify light elements (O, C) you need standards, standardless analysis is not reliable.
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I am working on 2D nanosheets. During the SEM-EDX and XPS analysis, I got too much difference in atomic percentage.
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The probe depth of XPS is about 10-nm which is a surface sensitive technique whereas EDX can vary from 1 to 3 microns - "bulk" analysis technique. The thickness and homogeneity of elemental distribution in the sample will thus cause different results by the two techniques.