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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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Most FESEM labs can coat a specimen with carbon instead of Pt or other metal. You may want to repeat your analysis with another, carbon coated specimen.
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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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Dear all,
I've acquired EDS maps during SEM analysis using an Oxford EDS device. I would like to know if there is a software which allows me to process these data (create scatterplots, compare element peaks, etc) or at least which allow me to convert these databases into .eds files. Could you please help me?
Thank you very much for your availability in advance,
Ignazio
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Dear all,
We have just published this work on the development of Datamuncher Gamma, a new software for the analysis of SEM-EDX maps.
Regards
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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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When temperature increases, it causes fading in organic matter and impurities
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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.
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I have an AlN sample and the EDX data show me the at% of a single atom such as Al, N and O . In order to measure the at% AlN , I have to use the chemical formula 2AlN = 2Al + N 2 . should I use the at% of a single N or I have to calcualte the at% of N2 ?
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Quite a strange question. You have a mix of Al2O3 and AlN solid phases and you have no N2 molecules at all, if we say about solid films. So, the answer is: "use the atomic % of N".
Your problem, as I can understand from the data presented is a AlN film on Al2O3 substrate. Is it right?
If so, the EDX method is not good in this case: electrons with energies of more than 5 keV (EDX) penetrate quite deeply into a solid (more than 500 nm) and, apparently, you observe an analytical signal from both the film (AlN) and from the substrate (Al2O3). For an accurate answer, you need a depth profiling analysis using one of the methods: XPS, SIMS, AES, LEIS, RBS ...
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While elemental analysis of the canine uroliths by energy dispersive X-ray (EDX) spectroscopy; on weight basis, we have detected Gold (Au) 23.46% in sample 1, 28.25% in sample 2, 9.46 % in sample 3, 9.25% in sample 4 and 6.11% in sample 5. Is it a normal findings
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Non-conducting specimens for SEM should be coated with conductive material, gold is one of the most common coatings. Looks like operator of your SEM coated specimens with too thick layer of gold and forgot to tell you about it. If possible, coat specimens with carbon. Do not pay attention to amounts of C, O and other light elements in your "quantitative" analysis, they are wrong.
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After putting the PEO coated glass substrate into the oven and subjecting it to a temperature of 180 degrees, it obtains a haze on the glass. A peak Si was observed after EDX analysis. Is there any possibility that Si is in the polymer or the observed peak coming from the substrate?
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Si is one of the constituents of PEO. Refer
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I was carrying out RAMAN Spectroscopy for MOFs. I have been carried out the XRD and EDX analysis for three samples synthesized by a different protocol. The crystal structure and chemical composition were the same for all three samples. When I performed RAMAN spectroscopy for these samples; I found one sample was Raman active while the other two was not showing any results. I performed the experiment by varying acquiring time and laser power for many times. But the results were the same. Please tell me the possible reasons?
Thanks
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If the Raman modes are collective (i.e. non-localized to a functional group), they are sensitive with respect to the crystallite size. I don't know how MOF modes look like, but you can check that out.
In principle, XRD should also be somewhat sensitive to that; do the reflexes there have the same width for all samples?
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a sample is a piece from a fuel element containing fuel exposed in nuclear reactor. We cut transversely the fuel element. what is happen with spectrum if the uranium emit gamma rays?
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you can do this. I assume that there is no Uranium in the sample iself.
So the sample will not still emit x-rays or gammas due to Uranium radiation.
Nevertheless you should perform two measurements:
a) perform EDX analysis with electron or x-ray beam OFF ---> spectruma
b) perform EDX analysis with electron or x-ray beam ON ---> spectrumb.
your net EDX spectrum will be netEDXspectrum = spectrumb - spectruma.
Please take care that the measurement times are equal.
Good luck
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Extracted chitin was subjected to Kjeldahl method, the result of nitrogen level obtained was 1.7 % ; however, EDX elemental analysis present various values of nitrogen form 3 to 6 %.
How can we explain this difference?
is each method present specific meaning of percentage?
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Proper quantification of light elements (such as N) by EDS is a tough task. It requires use of standards and good understanding of the technique. I believe that your results (as well as results from the paper you mentioned) were obtained by means of standarless analysis, which produces huge errors in light elements analysis. If you need bulk analysis of light elements (not a microanalysis, where EDS excels), use other methods, discard EDS results.
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Currently working on an alloy which demands to understand the characteristic morphology of each element and the mixed sample (contains more than one element). The peak of one is lower though their peaks could so close. Is there any technical way of analysis?
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Just because peaks have similar emission energies doesn't mean they have the same cross section. Please perform a stoichiometric analysis of your data (many EDX machines come with recommended parameter sets for that) and check whether there is an actual contradiction between values that you get from analyzing different peak pairs since with the information you gave us so far we can't tell whether there is an actual problem in the first place.
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I have EDX results and I want to caculate clinoptilolite formula. How I can do it while this mineral have smoewhat diffren ideal formula with variou amount of alkali and alkali earth metal.
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We can't measure it directly from EDX. It's only give us the stoichiometric concentration of the composition.
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I'm doing SEM/EDX for nanofiber with some additives and EDX results change from time to time for the same sample. Also the results are not consistent with the amounts of materials I use in my experiment. I'm thinking about test period, is there specific time requirement for the test? Is the time controllable or it's automatically determined by the device? And if detection period changes, will the results be the same or it is updated with time due to enhanced detection??
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Of course, the acquisition time is affecting the results:
1. Obviously, there is just a statistical effect: number of counts. The columns in the histogram are "jumping", then become stable. Just the law of large numbers.
2. Beam damages. The beam destroys the sample. This is especially important for thin samples (films, coatings, etc).
3. Carbon deposition under the beam. Even the purest chamber has some carbon contamination (SEM users know this annoying effect very well - dark spots).
4. Charging. Including local degradation of conductive coating.
Thus, in ideal world it would be easy: more counts, higher precision. But the real physical world is more complex. Experienced operators can choose the most optimal parameters of analysis. Sometimes, it is a kind of art.
Good luck!
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I have used an adsorbent. In FTIR analysis I was found carboxyl, hydroxyl, thiol and amino group in adsorbent. But in EDX result, the elements that can be detected only C, O, Na and S.The N element was not found.
Do you have any idea why this is happening?
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Dear friends, pleas stop this idiocy about non-detecting light elements. C and O were detected. Try to comment on things you know.
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I have done EDX analysis of welded joint of AA6082 T6 and AA6061 T6. Oxygen and carbon is found in the spectra. What are the causes for the same? Is it error due to some problem in sample preparation or any traces of air during testing.
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Dear Sachin Jambhale,
the problem you report is quite common and may originate from the material itself, from the environment and other surrounding (even the microscope itself, see ttps://onlinelibrary.wiley.com/doi/pdf/10.1002/sca.1996.4950180402) as well from the sample preparation and storage:
1) carbon contamination- the source of carbon can be from any contact with organic upon preparation or even from the air. Any organic contamination tends to form hydrocarbon under the electron beam on the sample surface, the amount of which can increase within the measurement you perform. It is very common effect in SEM and/or in (S)TEM. The most important is to clean properly the sample (plasma cleaning etc.).
2) oxygen - for many alloys, especially Al alloys it is very difficult to avoid it, since Al will passivate at the first possible contact with oxygen, unless one use a protective gas environment or very high vacuum, which is very difficult to realize (because the sample can not see oxygen at any moment between preparation and investigation) otherwise, just accept it is there and in the case you want to quantify the EDX data, keep it in mind and make corresponding corrections (especially important for TEM samples, for which material surface to volume ration gets significant).
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Since titanium (L) and nitrogen (K) peaks are very close and overlap in EDX spectrum (in TEM, 200kv), how the presence of nitrogen according to the EDX result in one grain of polycrystalline material can be verified ? How nitrogen (K) peak is seperated from titanium (L) peak?
thanks in advance
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This link could solve your doubt
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If using EDX with TEM, as opposed to the SEM, provides higher spatial resolution, why is EDX typically used with SEM?
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  • SEM specimens are much easier to prepare and they are lees artifact prone.
  • For EDX quantification bulk specimens (SEM) are better suited than ultrathin ones (TEM).
  • There are more SEMs around than TEMs.
  • For proper EDX usage it should be not TEM, but STEM, and most TEMs are not equipped with scanning capabilities.
  • If you use the same ultrathin specimen for both STEM and SEM, you'll have about the same spatial resolution (but of course imaging for STEM will be much better).
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I want to do compositional analysis of doped colloidal CsPbBr3 nanocrystals, by STEM-EDX.
However, even for short exposures, the electron beam induces carbon buildup on the sample, which dominates the EDX signal, and it becomes impossible to measure anything else.
Can someone indicate if and how they managed to do this type of measurement? Is the carbon buildup due to the organic ligands which are not attached to the nanocrystals? is there a simple way to remove them form the solution, to enable the measurement? Please note that I am not doing the measurement myself, so my knowledge of the technique is not very extensive.
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I would expect that you can detect the elements in the sample. Especially because you have high atomic numbers, the X-rays are hardly absorbed by carbon. The other condition is the energy used. To excite the sample volume you need low energies. To excite the elements you need high energies. I assume, you try to detect the M-lines or L-lines. The best chance, I believe is to look for the Pb-lines due to their high absorption you need a lower sample thickness. The M-alfa energy is 2,34 keV transition energy (so you need only 5 keV excitation) or L-alfa (10,5 keV). This is well to excite with 15 keV electrons. With such energies you penetrate the carbon layer and the X-rays do so. Perhaps it helpes.
With Regards
R. Mitdank
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Using only EDX it is not possible to distinguish between pyrite and marcasite, which, although they have equal compositions, have different crystalline structures. Or silica from quartz. I wonder if using the EBSD technique it is possible to differentiate one from another.
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Thank you very much, I apprecite it
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I am studying ephemere lake and playa. is it possible to make quick look analysis of salt sample taken with MEB witout EDX.
please find in attached sample of MEB photo.
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Just a little hint: MEB is SEM in English (that would attract more people who answer).
When you say you want to analyze the SEM without EDX: What do you want to know? From the image you can see that you have some 90° angles which would be expectable for NaCl and all other kinds of cubic structure salts, but of course the chemical composition is not available without EDX/XPS or maybe also a mass spectrum of your water sample.
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what is the difference between Element Wt% and Atom wt %?
how to find the concentration of particular element?
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please check the attached pdf.
have a nice day.
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On the surface of a WC piece a special metal is coated. The thickness is not known.
Is EDX able to detect the coated material on the WC surface? Must the coated layer have a certain thickness in order to be detected?
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Hello Vadim, Suntan and Simone,
many thanks for valuable information. I will check all your suggestions.
Have a nice day
Kim
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Hello,
I would like to ask whether normally Cu from a Cu grid is mapped on target samples on TEM-EDX images. I measured superparamagnetic zeolite samples by a TEM-EDX few times. Every images had Cu mapping images only
on the zeolite samples. I believe the Cu mapping images from the Cu grid as a background, because the samples do not have any Cu.
Do you know whether superparamagnetic samples affect to TEM and EDX? The superparamagnetic particles are Fe3O4.
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Cu background is a usual thing.
Mapping is not really good analytical method. Acquire spectra, from a spot at a specimen, and another one from an "empty" space and compare them.
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Dear researchers,
I have some multiport extruded tubes with a certain white precipitate visible on the iner side of the tubes and would like to know a way to determine what that precipiate is.
During extrusion the aluminium multiport tubes are passed through a water quench to cool them down from an temperature in excess of 500°C to about 40°C. In some cases when the water enters into the ports of the MPE tube due to porosities a thin layer of white precipitate is observed which is mostly aluminium hydroxide. In severe cases a considerable amount of white powder can be detected. After performing an XRD on the white powder it was found to bayerite.
Also anodic dissolution of aluminium around the Al(Mn,Fe)/Al(Mn.Fe)Si precipitates was observed when some samples were analyzed under the SEM. Very minute quantities of oxygen could be detected with the EDX analysis on the SEM but these measurements cannot confirm the exact composition of the precipitates.
Is there a quick way to determine if the precipitate on the surface of the tube is Aluminium hydroxide?(without the need to perform XRD or any other time consuming analyses) And can any other type of precipitate that can form under these conditions?
Would be grateful for your inputs and suggestions.
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There is only one way to be certain. Solve the structure of the material. Scrape the surface onto a carbon coated grid and use micro diffraction techniques in a tem or backscatter diffraction techniques in an sem. The material may be beam sensitive so good luck but there is only one way to be certain, solve the crystallography.
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I have synthesized Ru-doped mesoporous carbon. At low composition I could not get any XRD peak for Ru, however HAADF-TEM shows monodisperse Ru particle in the carbon substrate. As single atom does not give any XRD spectra, so are there minimum crystal structure at which XRD fails to give any spectra? Noted that EDX mapping and XPS show 0.2 at% of Ru.
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Please go into the Scherrer equation and roughly calculate the peak width dependence on the crystallite size by your own. In your case of particle size of about 2nm (assuming crystallite size is also about 2nm) you will end up at about 0,15rad peak width in 2 theta; i.e. about 8°.
You know that when peak width is increased the peak height goes down. Thus at your small Ru concentration you will hardly see such a peak.
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The rice straw biochars were prepared under oxygen limited conditions in muffle furnace at 350⁰ C (350BC) and 550⁰ C (550BC) and that prepared under nitrogen conditions at 400⁰ C (CBC). From CHN analysis of rice straw and its biochars, 40, 52, 29, 26% carbon was observed in rice straw, 350BC, 550BC and CBC, respectively. From EDX analysis , 20% carbon was observed in rice straw and carbon was absent in all the biochars. The silicon content was 38, 17, 24 and 25% in rice straw, 350BC, 550BC and CBC, respectively. Can someone give reliable reason, why CHN and EDX give contrast results and carbon was absent in all the biochars in EDX analysis?
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It might be due to ignorance of the peaks for C while choosing the element peaks for EDX spectra.
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Hello, I am doing x-ray dispersive (EDX) analysis for Inconel 718 alloy. I have noticed that the elements with higher concentrations in Inconel 718 ( i.e: Nickel- 53%) is providing better accuracy than elements with lower concentration (i.e: Mo- 3%) when I compare the concentration result against available literature. From here, can I come to a conclusion that EDX provides more accurate results for elements with higher concentration in a sample? Thank you!
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By edx you can determine the elements mostly located in the surface of the sample. If you are sure that the sample is homogeneous throughout, then this method will be more reliable.
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Dear experts,
I am struggling to calculate the accurate weights of starting precursors to represent the formula Mg0.95Ni0.04Cr0.01O. The precursors are:
1. Mg(NO3)2.6H2O (M.W = 256.4 g/mol), M.W of Mg is 24.305 g/mol which represents about 9.47 %.
2. Ni(NO3)2.6H2O (M.W = 290.8 g/mol), M.W of Ni is 58.69 g/mol which represents about 20.18%.
3.Cr(NO3)3.9H2O (M.W = 400.14 g/mol), M.W of Cr is 51.996 g/mol which represents about 13 %.
I used 0.5 M (0.025 mol) by disolving the precursors in 50 ml water. To represent the chemical formula above, I variate the precursors amount as follow:
1- Mg(NO3)2.6H2O , 0.5 M x 0.95 = 0.475 M, (0.02375 mol). 6.0895 grams, to represent the amount of Mg, 6.0895 x 9.47% = 0.57722 grams,
2- Ni(NO3)2.6H2O, 0.5M x 0.04 = 0.02 M, (0.001 mol). 0.2908 grams, to represent the amount of Ni, 0.2908 x 20.18% = 0.05868 grams.
3- Cr(NO3)3.9H2O, 0.5 M x 0.01 = 0.005 M, (0.00025 mol). 0.100035 grams, to represent the amount of Cr, 0.100035 x 13% = 0.01299 grams.
by summation and dividing the results, I got , 89 % Mg, 9 % Ni, 2 % Cr.
Therefore, when I consider the wt%. , the calculated values do not represent the formula (Mg0.95Ni0.04Cr0.01O) becuase I use the weights of metal nitrate precursor not the bare elements Mg, Ni and Cr. Further, both Ni and Cr are heavier than Mg.
I believe that the quantitaive EDX results will give me very different values.
I used sol-gel method to produce the gel and heat treated at 400 C.
I hope I will get help.
Thanks in advance
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Mohammed M. Obeid Thank you and good luck to you too for your future work
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As we know that the if the atomic percentage of copper is 66.85 Cu and Se is 33.15 , then the composition is Cu2Se. Is there any formula to calculate the elemental compositions of Cu3Se2,Cu5Se4,Cu7Se4 ...? If the atomic percentage of copper is 78.50 and Se is 21.50, then what will be the composition ? 
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Dear Prof.Ian which parameter we use in the EDS report for calculation of the composition the wt% or at% and how reliable is this method to know the composition
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Hi everyone, hope you're all okay. So I have some questions/doubts about eds mapping. Just some notes first: I always use the correct accelerating voltage to excite the elements I need, always use correct probe current to have a good dead time and counts and not forgetting to check the working distance, and last but not least I always try to perform eds with flat surface and polished (but sometime this is not possible).
My doubt is: sometimes when I do eds mapping the distribution of the elements appears dislocated. The pixels dislocates not corresponding to the SED image. Why this dislocations happens?
Besides the deslocated pixels, most maps is very "noisy", I've changed the resolution already on the software to 1024 instead of 4080.
Peform map in 4080 resolution takes too much time. So I would be very grateful if anyone give me some tips on how to improve eds maps.
Thank you for the attention
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One of the most common causes of mismatches being images and maps is sample movement. This may be caused by loss of volatiles from the sample (which will cause it to shrink) or, most often, the effects of temperature changes. These may be induced by the electon beam or through environmental changes - try letting the sample equilibriate in the beam for a while.
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The carbon composition of steel stock is given as 0.06wt% and the EDX analysis of the ferrite phase gives 12.7wt% of C. How do you relate the two wt%s in terms of relative abundance? This situation is shown as an attachment below.
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EDX is not the right technique to measure trace elements and it is really very approximate to measure carbon. The carbon detected here is probably located only on the surface of the sample.
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I need to decide which SEM (with EDX) model to buy. I am told that in going from 100 to 200 nA, there is not much to be gained. I just needed to cross check this claim and educate myself about specific cases where it is advisable to buy one vs another.
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100 to 200 nA? Are you sure? It is huge even for a FIB (typically max ion current is about 100 nA). The spot size will be terrible (micrometer?!). Most common parameters for EDX - current from 0.1 to 1 nA, HT from 10 to 30 kV, almost all normal SEMs meet these conditions.
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I had a Galfenol (Fe:Ga, 81:19 %at.) target made for sputtering, when I received the target I sent it for an EDX analysis and the results came back as Fe:Ga:C (60:11:29 %at)
I am curious about other people's experience with this type of target (or perhaps Fe), is this what one would typically see for the EDX and the C content ignored as a surface contaminant?And is a long pre-sputter time just used to ensure clearing of the C? And I am aware that the EDX itself can be the source of C in the readings.
Or do I have a questionable target?
The follow up would be the films, to ensure that they do not end up being a ternary FeGaC alloy.
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I second a suggestion to analyze at two different kVs, to check if C is a surface contamination. Then - analysis of a target. It is not unreasonable to see 29% at as a contamination, but your SEM should be quite dirty.
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I am curious if the surface roughness of a target is considered an important factor for sputter deposition, because if my target is rough I think there is a higher chance of contaminants becoming trapped in small pores, for instance organic contaminants like carbon.
If the surface roughness of the target is minimal and very smooth there is less areas/pores where these could become trapped.
For example, I had an EDX analysis done on a LiNBO3 off cut which I clean in acetone, it had a polished smooth side, and an unpolished rough side.
The smooth side came back without any other additional elements listed, but the rough side showed traces of C, K, Cl, in some of the points that were taken.
And I am curious for sputtering, if my target surface, for a new target, is not a polished surface, and I see other elements from the EDX analysis for this target, I expect I run the risk of deposited films of compositions other than what my target is supposed to be.
I understand pre-sputtering is used to clean a target surface before deposition, and some people suggest plasma cleaning in O2 for some time also to minimise contaminants.
But do people also polish their targets surface so that it is smooth to minimise pores where contaminants could become trapped?
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I agree with the Dr. m. Toma, because presputtering time will decide the concentration of contamination on the target surface. The self made targets are rougher than the paid targets.
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I have EDX analysis of a sample. it gives wt% of the elements present in the prepared oxides. can i convert this wt% to mole % to verify the proportion in which initial precursers were taken to prepare the sample.
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Dear Rajni Vats,
Formula to convert wt% to mole %
Example:-
Calculate the molar wt of each oxide you want.
e.g. BaO
Atomic wt of Ba + atomic wt of O = Molar wt of BaO
  1. Divide all weight percentages by the molar weight of the oxides.
  2. Sum the answers obtained under 1.
  3. Molar percentage of an oxide is equal to the answer obtained under step 1. divided by the answer under step 2, times 100.
I hope the information will help you.
With Best Wishes,
Samir G. Pandya
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I thought Calcium peaks are expected to appear in 3.6 eV only, but why does myne appear in other eV as well?I only understand Each peak represent the presence of element for that particular energy. How do i know which one is KAlpha or Kbeta
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Different peaks for same element in EDAX is due to excitation of atomic energy level of respective element under incident energy of SEM/TEM. This will bring possiblility of XRAYS in energy range of different energy level i.e. k-alpha, L-alpha, k-beta, etc. It is depend on sample stability, incident energy of SEM /TEM to make proper excitation to get Xrays.
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Someone sent me an EDX graph in which there are different peaks for gold at different region having different intensities. i am confused that how is it possible?
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EDX measures X-rays that are emitted from an atom after a core electron has been kicked out. The X-ray is emitted when an outer shell electron (with higher energy) relax into the "hole" left by the electron that was kicked out. The energy of the X-ray is then determined by the energy difference between the outer shell electron and the hole. The outer shell electron jumps from a higher energy state to the lower energy state of the hole - the energy difference leads to emission of a photon with that energy - the X-ray. Since the outer shell electron can come from different shells with different energy, X-rays can be emitted with different discrete energies, which gives rise to a number of different peaks in the EDX spectrum. You may be able to see labels on the different peaks that indicate what transition occured to release X-rays at that peak.
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I have been sputtering an alloy of Fe Ga, when I get the EDX results of my film back there is a larger percentage of C present in the results, which is unexpected. I did notice that as the film thickness increases the relative percentage of C decreases.
And an EDX of my target now shows the presence of C on it, I think this should just be the surface of the target that is affected.
From the target manufacturer I have a document of the composition analysis of the target which does not indicate any trace of C within my target.
I think it is likely coming from the chamber, the target shield and clamps have blackened over time, during the course of heating during the process. Might that be the source? A dark ring starts to appear around my target after sputter.
My understanding of the sputtering process is that it should essentially be cleaning away the surface layer of the target during the process as the ion bombardment occurs. So I am not quite sure what may be happening here.
Any thoughts on this and possible remedies would be appreciated
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