Science method

Elemental Analysis - Science method

Elemental analysis is a process where a sample of some material (e.g., soil, waste or drinking water, bodily fluids, minerals, chemical compounds) is analyzed for its elemental and sometimes isotopic composition. Elemental analysis can be qualitative (determining what elements are present), and it can be quantitative (determining how much of each are present). Elemental analysis falls within the ambit of analytical chemistry, the set of instruments involved in deciphering the chemical nature of our world.
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When EDX can be used under all conditions, why XRF need to be used. Or why people buy XRF instruments.
Even though both the techniques use different sources viz., electron (EDX) and X-ray (XRF), both the analysis are dependent on their characteristic X-rays for elemental analysis. Why their is difference in the detection limits and sensitivities.
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Also see my answer to your other question.
EDS refers to energy-dispersive spectroscopy. The E does not refer to electrons. Several vendors sell XRF systems with EDS instead of WDS (wavelength-dispersive).
EDS collects in parallel and cheaper but is limited in count rate and resolution. That makes the detection limit poorer. For the SEM, I quote a detection limit around 0.1 wt%, but that depends A LOT on your setup.
EDS is often used with an SEM beam for excitation. That permits microanalysis. XRF always(?) uses an x-ray beam for excitation. That virtually eliminates the background and improves detection to the ppm range. Unfortunately, it is not a micro technique.
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I conducted elemental analysis for some agricultural wastes for use in the production of bio-oils. The C,H,N,S,O have been determined but need to calculate the H/C and O/C ratios.
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The atomic mass of carbon is ~12 AMU and that of hydrogen is ~1 AMU, the C/H ratio is calculated by multiplying the atomic mass of each element by the number of atoms of that element, and dividing the result for carbon by the result for hydrogen. It is done by doing. say if value of carbon content is 67% then it should be divided with atomic weight of carbon which is 12 which should be 5.58. In similar way for N, H and O all the % calculated values should be divided with their respective atomic weight and then with theses calculated values ratios should be calculated. So, to calculate the molar ratio of H/C, you can do by [%H/1(g/mol)]/[%C/(12g/mol)]. For example: %H = 1, %C = 80, so molar ratio of H/C = 0.15.
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We are currently developing a BFT system. It is necessary to measure the C:N ratio level in BFT. Imhoff cone techniques are used only to observe floc density.
However we prefer to measure the C:N ratio in the BFT rather than using elemental analysis. Can anyone suggest if there is a device or kit available?
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There are C/N analysers that function well
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Hello,
I am trying to find the H/C effective ratio from waste cooking oil and LDPE feedstock. i conducted already the elemental analysis and got the element percentage. I found the formula:
H/Ceff= (H-2*O-3*N-2*S)/C
however this are moles, may i know if someone have experience with this or know how to find this ratio?
Thanks in advance
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Hello,
Absolutely, the question you've raised about calculating the effective H/C ratio is indeed quite pertinent when it comes to pyrolysis, especially with feedstocks like waste cooking oil and LDPE. The H/C_eff ratio gives us valuable clues about the kind of products you might expect from the pyrolysis process—be it bio-oil, syngas, or char. It's all about understanding how hydrogen and carbon play together in your feedstock, which is crucial for tailoring the pyrolysis process to get the results you're after.
Now, I'm curious about a few things regarding your experiment that could help me provide you with more tailored advice. For starters, how did you go about preparing your samples for the elemental analysis? Also, the presence of certain elements like oxygen, nitrogen, and sulfur can really change the game due to how they interact with hydrogen. Have you noticed any specific compounds or peculiarities in your feedstocks that caught your eye? Sharing these details could really help in dissecting the H/C_eff ratio calculation and ensuring you're on the right track for your pyrolysis project.
Let me know if you need to take a look on one of the papers I produced regarding this topic that maybe can help you.
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Reaction Yield= mpurified*w%/n*MPb
where mpurified is the mass of the dried quantum dots, w% is the mass
percentage of lead (28.74 %) [by inductively coupled plasma optical
emission spectroscopy (ICP-OES) elemental analysis], n is the number of
CsPbBr3 quantum dot moles, and MPb is 207.
n should be the moles of Pb precursor according to "The reaction yield is assessed in terms of Pb present in the DBSA-QDs compared to the Pb precursor."
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Yield (%) = (Number of QDs obtained / Number of QDs synthesized) * 100
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mineral element analysis
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Can you elaborate please: What species of plants are you working on, what elements do you wish to examine, what equipment and reagents do you have in your lab?
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WHEN WE DONE THE ELEMENTAL ANALYSIS OF THE BLACK SPOT AREA THE CHROMIUM CONCENTRATION INCREASES. CAN ANYONE PLEASE TELL ME WHAT IS THE REASON BEHIEND THE INCREASE IN THE CHROMIUM CONCENTRATION PARTICULARLY AT THE BLACK SPOTS.
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Уважаемый господин,
Спасибо за ваш ответ.
Не могли бы вы вкратце объяснить причину окисления и то, как это окисление приводит к увеличению концентрации хрома с фактических 12 % до 25 % в этом черном пятне.
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Can you please explain the type of steel mentioned in the elemental analysis above
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Macdenis Onyekachi Egbuhuzor Thе composition you providеd corrеsponds to a typе of stainlеss stееl known as "Austеnitic Stainlеss Stееl." This typе of stееl is charactеrizеd by its high lеvеls of chromium and nickеl, which contributе to its corrosion rеsistancе and ability to withstand various еnvironmеntal conditions. Thе spеcific composition you mеntionеd falls within thе rangе of typical valuеs for austеnitic stainlеss stееl.
It's important to notе that thе dеsignation of thе stееl within thе austеnitic stainlеss stееl catеgory may vary basеd on additional еlеmеnts and spеcifications. Thе composition you providеd includеs thе following еlеmеnts:
Carbon (C): 1.03%
Silicon (Si): 3.73%
Manganеsе (Mn): 2.5%
Nickеl (Ni): 5.41%
Phosphorus (P): 0.037%
Austеnitic stainlеss stееls arе widеly usеd in various applications, including construction, automotivе, and food procеssing, duе to thеir еxcеllеnt corrosion rеsistancе, formability, and durability. If you havе morе spеcific rеquirеmеnts or if additional еlеmеnts arе prеsеnt in thе stееl, it may bе nеcеssary to rеfеr to industry standards or consult with a matеrials еnginееr for a morе prеcisе classification.
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Porphyrin-fullerene dyads have been there for quite a few decades now and have applications in diverse fields ranging from medicine to energy applications, and as energy storage devices. A variety of methods are available for accurate characterization of such dyads, such as, 1HNMR, Mass Spectra (HRMS or MALDI-TOF), XRD among others. While it is understandable that 1HNMR is a mandatory criterion in combination with mass spectra to characterize the structural features of such systems. The question is what role does 13C NMR play here? or HRMS? These are macromolecular systems and getting accurate 13C spectra is a near to impossible task, the same applies to HRMS as well, and elemental analysis. There are numerous publications on the synthesis of porphyrin-fullerene dyads which do not report, in other words cannot report analysis results such as 13CNMR or elemental analysis or HRMS. Is it fair then to impose 13CNMR/HRMS/elemental analysis as a mandatory criterion for complete characterization of such macromolecules? Shouldn't the standards be different than that for small molecules considering the sheer size and structural complexity? I believe a clean NMR and MALDI-TOF analysis is more than sufficient to establish the structural identity of such molecules. I would love to know the opinion of the scientific community on this matter.
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Size and Complexity that's means Macromolecular systems are indeed larger and structurally more complex than small molecules. Analyzing them with techniques like 13C NMR can be challenging due to signal dispersion and sensitivity limitations.
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For electrodeposition of metals on a small SS disk at trace level I used XPS to know whether the the deposition was in metallic form or it was in compound form. In XRF, I did not get such information. Will you please explain me the reason behind it?
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Thank you very much for your nice explanation and the reference of your book mentioned. I shall try to refer your book once I get it.
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I need, how many elements are present in the sample and how to find out from the sample.
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XRD maybe and then NIR (for organics)? I presume you want methods that are non-destructive.
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Do anyone understand how the author determine the Chemical formula and vacancy from the elemental analysis?
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ICP elemental analysis can be used to determine the presence and concentration of metal analytes in a sample. From the concentrations obtained by ICP-AES, it is possible to calculate the chemical formula of a compound.
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If instruments are good please mention the name.
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Mossbauer spectroscopy may be of assistance in determining the iron oxidation states.
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According to my view, even the mere opening of a drawer or a cupboard is already damaging to cultural remains. The shock of opening a drawer, the changing environment between the inside and the outside of a drawer, as well as a sudden light that falls on an artifact that has been in the dark is damaging to any item, especially to parchment, papyrus and paper.
When it comes to 'taking a sample' needed for applying a analytical technique to an artifact, one can only speak of less and more destructive, because destructive it is.
For example in Neutron Activation and Petrography, one needs either an amount of 80 mg of pottery powder or a thin-section before submitting the sample either as powder or as a pellet to a nuclear reactor or to a glass slide to be looked at under a microscope.
I think that the formula "non-destructive sampling technique" was invented by scientists to obtain samples they needed from a curator or conservator. I, therefore, suggest to omit the word "non-destructive" from the Cultural Heritage vocabulary.
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I think we should make a difference between sampling, materials and techniques when talking about non-destructive or non-invasive.
Taking a micro-sample on an artefact is invasive and destructive, while its analysis can be non-invasive and non-destructive. Also, the difference between invasive and destructive should also be taken into account. Invasive means that there is an interaction between the material and the technique, while destructive means the material is destroyed = cannot be re-analysed.
Based on that, some techniques are invasive, but non-destructive.
Also, semi-invasive techniques do not exist (at least in my opinion), while semi-destructive techniques exist. A preparation technique, such as cross-section for example, is semi-destructive. During preparation, part of the sample is polished = destroyed, but the rest of the sample remains whole and could be re-analysed (extraction from resin can be discussed). We can argue about how much invasive this preparation is then, but it largely depends on the method of preparation/protection.
When the cross-section is analysed under an optical microscope, the destructivity depends highly on the material we are observing (exclusion of staining). For most cases (hard substrates, inorganic materials, resins, some organic materials as well), it is non-destructive and non-invasive.
When SEM is used, the same principle can be applied, which means we will have a non-destructive, but invasive analysis. Again, it depends on the material analysed.
In conclusion, the terminology should be carefully explained, and what is determined as non-destructive, semi-destructive, destructive (same for the invasivity) should be carefully described.
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I'm doing an elemental analysis of soils using an XRF Analyzer, the results obtained are in ppm. My question is, can I directly convert values from ppm to mg/Kg of soil?
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I mean, identifying the presence of some complex unknown compounds, not just finding the crystalline phases!
Moreover, I have the XRF result of the mentioned compound (elemental analysis) and the existence of crystalline phases. However, I need to know if it is possible to characterize the probable complex compositions.
Thank you in advance for your help
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For crystalline compound, XRD is the best, but you don't know this compound has crystallinity region or no
there for you need analysis with Elemental analysis and XRF
second time you know which instrument is the best
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Dear scholars,
I have a database with 100 geolocated samples in a given area, each sample contains 38 chemical elements that were quantified.
Some of these samples contain values Below the Detection Level of the instrument (BDL), clearly, when we have 100% of the samples with BDL values there is not much to do, but what can be done when, for example, when there is only 20% BDL, what do we do with them, with what value do we replace a BDL sample?
Some papers show that a BDL sample can be replaced by the detection level (for the instrument's minimum detection level for that chemical element) divided by 0.25, others show that you have to divide it by 0.5... What would you do in each case, and is there any literature you would recommend? If it matters, I am mostly interested in Copper and Arsenic.
Regards
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What fraction of values below BDL is acceptable.
Why are you making the measurements? The why determines what is acceptable.
If you are concerned about an upper limit, then BDLs are of no concern.
If you are concerned about a lower limit, it will depend upon the nature of your concern.
There is no recommendation. There is no rule of thumb.
You decide from the criteria associated with WHY if you have enough information.
Too many BDLs might mean you need a different technique, but it always returns to WHY.
If , say, a customer wants an answer at each location, use the actual result and note the uncertainty. The result is usually meaningless, because of the high uncertainty.
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How do I calculate the ratio e / a (eletron/atom) for a metallic alloy with more than two elements?
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e/a for a multi-component alloy can be defined as the weighted average from e/a of the constituent components:
e/a=SUMM[Ci*(e/a)i ]
where ci is atomic percentage of the ith component
(e/a)i for the individual element
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I want to do plant experimental studies of wheat. Prior to this, I have done soil elemental analysis of primary nutrient and organic carbon. In 1 gram of soil , they are as follows:
N = 0.007 %
P= 0.00024 %
K= 0.00002 %
Organic carbon = 0.0025%
Organic matter = 0.0043 %
pH = 6.5
Now, I want to compare that is this alright to start the experiments or they are nnutrient deficient soil? How to compare with recommended level of soil. Kindly help
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You should search for information in specialized journals. E.g.:
J. Plant Nutr. Soil Sci. 2020, 183, 705–717 DOI: 10.1002/jpln.201900590 "Bioavailability of macro- and micro-nutrients chemically extracted in acidic soils for wheat"
ZJ
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Nitrogen peak areas of 6 out of 10 blank samples (synthetic quartz) are below the lower working range. I am afraid the estimate of the limit of detection (LoD) might not be realistic.
The mean value of the 10 blanks is 41.5 (42 is the lower limit of the range).
"In case the noise peak in the blank sample is not measurable, the peak relative to the lowest concentration of the calibration curve can be used, provided its value is comparable to LOD. In this case, the LOD will be simply 3 times the standard deviation of the lowest concentration level, as mean blank is considered as zero."
From: Bratinova, S., Raffael, B., & Simoneau, C. (2009). Guidelines for performance criteria and validation procedures of analytical methods used in controls of food contact materials. JRC Scientific and Technical Reports, EUR, 24105.
Does that mean I can take the mean blank value to be 42 since that is the lower noise peak for N and to calculate LoD add three times the standard deviation of the 4 readings that are above 42?
Please give me your thoughts on this. I am a student trying to understand more about the analytics behind elemental analysis.
Every reply will be greatly appreciated.
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One possibility is to spike both blank and test samples with certain amount of the same item/material which has to be measured and thereby increasing the concentration and detection limit.
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Hi everyone, I want to obtain the elemental composition of a thin film coated on a gold surface. What I need to prove is that the presence of sulphur in the thin film. Which analysis gives better proof? SEM-EDX or XRF?
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let me first summarize some facts:
i) 'thin' film containing sulfur (S) on top of gold (Au) layer
ii) S containing film:
S K-edge: 2,47keV
S fluorescence lines:
S K-alpha: 2,3keV
S K-beta: 2,46keV
iii) Au substrate:
among others;
Au MIIIedge: 2,74keV
Au fluorescence lines:
Au MIIINIV: 2,39keV
Au MIIINV: 2,41keV
Data were taken from J. A. Bearden tables:
conclusions:
a) The energy position of the S K-beta line is about 50eV above the Au MIIINV line; but due to the limited energy resolution of the detector (assumed to be about 120eV) S K-beta will not be seen in the presence Au MIIINV.
b) The energy position of the S K-alpha line is about 90eV below the Au MIIINIV line; but due to the limited energy resolution of the detector (assumed to be about 120eV) will not be clearly seen in the presence Au MIIINV.
c) thus the Au lines have to be omitted or extremely minimized.
There are two ways to do this.
i) avoiding, that excitation radiation will reach the Au stubstrate
and/or
ii) reduce the excitation energy to below Au MIII-edge energy.
XRF scenario:
In the case of XRF, you have to have x-ray photon excitation energies of above the K-edge energy of sulfur, which is at about 2,47keV. For a significant fluorescence yield you have to go to x-ray tube voltages of well avove 2,47kV, at least some 100V above. However, for the maximum photon energies of such an x-ray spectrum you will have penetration depths in the very low µm regime; thus the x-rays will also hit the Au layer beneath your thin film and will be able to excite the Au MIII core level, when the energies are above 2,74 keV.
SEM-EDX scenario:
In the case of electron excitation one will have sub micron penetration depths for the whole electron scatter cascade, when you deal with quite low primary electron energies*). The penetration depths of the primary electrons of such a beam is much smaller.
So there is a chance, that you will have only a small fraction of primary electrons, which will be able reach the Au substrate.
If one in addiiton restricts the electron beam voltage to below 2,74keV; there is no possibility to excite the Au MIII fluorescence.
Final conclusion:
a) XRF is, to my opinion, not suitable here, due to the strong S- and Au-peak overlap.
b) SEM-EDX may work, if the electron acceleration voltage is restricted to below 2.74kV (but well above 2,47kV).
Good luck an
best regards
G.M.
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I have synthesize Nickel cobaltite through various methods. I have gone through XRD and EDS, But I still wonder what preliminary test/characterization can be performed to support the elemental composition is 1 :2 :4 for Ni: Co: O.
I have to justify that Co is 2.
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I would not rely on EDS , EDX or EDAX or whatever abbriviation are used.
The reason is that the O-K-alpha has an photon energy of about 525eV.
This means that the escape depth and tghus the information depth of the O K-radiation in the presence of Ni and Co is quite small; only about a very few atomic layers.
The situation for the Ni and Co L-radiation is a bit better but not ideal as well.
So you are quite surface sensitive and thus you will get informations about the surface stoichometry of your sample. Any contamination of your sample surface by adsorption of O containing molecules ( e.g.by O2 itself or water) will give huge errors in the O concentration estimation relative to Ni and Co.
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How do I use the CHN methodology liquids? Does anyone have a paper that describing this methodology?
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Using Elemental Analyzer to measure Soil Total Carbon (STC), Soil total nitrogen (STN), C/N ratio, total sulfur content is a good technic. Sulfanilamide usually used as standard for machine calibration and after every ten measurements. How we can ensure the accuracy of the data after analysis?
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Through a pilot scale testing, which you can customize as per your need
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I have functionalized a material with an organic compound and performed different analyses such as TGA, XPS, elemental analysis (by EDS and varioMICRO) but I have a difficulty to determine the general formula. Is there any equation?
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Reconcile elemental analysis for all methods. Determine the mass average. Write a formula, such as water or hydrogen peroxide. You have determined 12% hydrogen and 88% oxygen. Write the unknown formula HxOy. Find the ratio x: y and, resulting in an integer ratio
12/1: 88/16 = 12: 5.5 = 2: 1. Hence, you have identified water, not hydrogen peroxide.
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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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Dear Experts:
In the absence of elemental analyzer and XRF, Is it possible to calculate composition of compound elements from the compound formula listed in crystallographic data?
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Dear Adnan Qadir thank you for this very interesting technical question. In my opinion single-crystals X-ray diffraction data cannot replace classical elemental analysis. Here is the main reason: The X-ray data will give you the exact chemical composition of the compound, but only for the crystal which has been measured. Quite often the bulk material contains only very few well-formed crystals, from which one of them is selected for the X-ray dffraction study. Thus the composition of this single crystal does not tell you anything about the chemical composition of the bulk material. In some cases only a by-product of the reaction crystallizes nicely, while the main product only forms a microcrystalline powder. In other cases the good crystals contain a different amount of solvent of crystallization. Thus when it come to publication of your work please keep in mind that the X-ray diffraction data are not a suitable replacement for elemental analysis.
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If there is any formula or software that can assist, please clarify.
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Can you please reword your question as it does not make sense.
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Is EDX-FS sensitive enough to quantify the available and total micronutrients (Fe, Mn, Zn, and Cu) concentration in soil and plant samples?
Is EDX-FS accurate in terms of nutrients/elements analysis when we compare it with wet-analytical methods?
Can carbon, nitrogen, phosphorus and potassium (both total and available form) be measured accurately in soil and plant samples using EDX-FS? And based on its results can we calculate fertilizers recommendations for the particular crop?
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Is EDX-FS sensitive enough to quantify the available and total micronutrients (Fe, Mn, Zn, and Cu) concentration in soil and plant samples?
Is EDX-FS accurate in terms of nutrients/elements analysis when we compare it with wet-analytical methods?
Can carbon, nitrogen, phosphorus and potassium (both total and available form) be measured accurately in soil and plant samples using EDX-FS? And based on its results can we calculate fertilizers recommendations for the particular crop?
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Yes, it is possible, especially in estimating phosphorus and some growth regulators
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For example in one research article the Elemental analysis values of COF-TpPa-1 ( Triformylphloroglucinol (Tp) (63 mg, 0.3 mmol), Paraphenylenediamine (Pa-1) (48 mg, 0.45 mmol) are as follows
Anal. Calcld. For C80O12N13H48 : C, 69.5; H, 3.47; N, 13.87; found : C, 65.7; H, 3.32; N, 12.71
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Dear Muzammil Hussain, If you have the software ChemDraw Ultra , then you can write down the molecular formula or the structure of the compound and the go to analysis window and click it . You will get the elemental analyses well as exact Mass of the compound.sis data . If you don't have it then from standard books you can get the exact average atomic weight of an element up to 4th decimal. Then manually it can be calculated depending on number of each atom present. From it you can calculate the percentage. For your compound it showed the following elemental analyses data as shown by Chemdraw
C80H48N13O12
Exact Mass: 1382.3545
Mol. Wt.: 1383.317
m/e: 1382.3545 (100.0%), 1383.3579 (86.5%), 1384.3612 (37.0%), 1385.3646 (10.4%), 1383.3516 (4.8%), 1384.3549 (4.2%), 1384.3588 (2.5%), 1386.3680 (2.2%), 1385.3621 (2.1%), 1385.3583 (1.8%)
C, 69.46; H, 3.50; N, 13.16; O, 13.88 %
You can verify the purity / authenticity of your sample by comparison with the experimental results
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I've prepared some metal composites based on transition metal oxides. How may I be able to digest the sample in order to have elemental analysis?
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I have great differences between duplicate digestions of sewage sludge, but only for some elements like Fe and P.
l use closed vessel microwave digestion with HNO3 and H2O2.
Usually the "failed" duplicates have a much lighter colour compared to the usual yellow solution and they have a fraction of the concentration for certain elements. Sometimes the same sample produces multiple failed duplicant, and sometimes none.
l checked the acid dispensers, the loss of mass during digestion and the microwaves, but no correlation so far.
l have trouble investigating the problem beacuse of its apparent randomness. l tried running a study on the effects of different digestion parameters with a sample that had previously produced the issue. But no major effect that is comparable to the main problem was discoverd.
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Hi there,
we want to press pellets from different soil samples (powdered in advance) in order to use them for total element analysis via XRF.
In advance, we tried to produce pellets from certified reference material which is very finely powdered. We used Licowax Micropowder as binding addidive but never got satisfying results after homogenization - there were always white dots (wax) remaining. We used both homogenization "by hand" in a mortar and homogenization in a Retsch Mixer Mill (30 min., frequency: 20, using agate balls).
Can anyone suggest a good way of preparing XRF pellets from reference material (e.g. sewage sludge) or natural soil samples?
Thank you in advance!
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You can use cellulose powder (10% wt/wt) as a binder to prepare pellets from soil samples for X ray fluorescence spectrometry (XRF).
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I am working on the development of an elementary impurities method for an API by acid digestion via microwave and ICP-OES analysis. [API = Amiodarone HCl]
However, at the end of the microwave program, I notice that a platinum / black solid is impregnated in the Teflon tube. I figured it could be the iodine from API composition, that is not soluble in acid reagents.
Has anyone worked with the analysis of elemental impurities for a compound with a high concentration of iodine and can you help me with this? (microwave digestion)
Could the solid on the wall of the Teflon tube be the iodine?
Would add AgNO3 for precipitation work in this case?
Would it be correct to let the solid form on the tube wall and proceed with a simple filtration of the solution?
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I suggest you look up the archives of the Plasmachem-L ICP discussion board.
There is a search function that should help you out in the first instance, and you can always subscribe and post a question if that doesn't help.
There was a useful thread back in March 2020 about just such an issue.
In general, Iodine and nitric acid don't get on well. Digestions should be alkaline.
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I synthesized some (metallo) porphyrins. I am now characterizing them by Mass spec and also confirming their purity by Elemental analysis. The values I got are a little deviated from the calculated values. What is the allowed limit of deviation for mass spec and elemental analysis in porphyrin chemistry? I will appreciate some references too. Thank you.
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With respect to Mass spectra, the mass error should be within 5 ppm (for ESI-HRMS). You can use the following website to calculate or you can do the calculations on your own. Those are simple enough.
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Following elemental analysis of two osteoma samples using XRF spectroscopic & MPAES techniques, I have detected Nickel in both the samples; whereas in native bone sample of the same species from same geographical area was found without presence of Nickel.
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There are many epidemiological studies that confirm the relationship between the contamination of toxic metals in human body and cancerous disease.
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After elemental analysis of the samples, carbon content of the charcoal was 102 (several repetitions were made, but obtained the same values), the equipment was tested with other samples of wood obtained coherent results (the equipment is working well). How can I adjust the elemental composition values since the sum of C,H,N,O and ash should be 100?
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If the CHNS analyzer doesn't work properly, you can verify the results by the TOC analyzer or you can check it by EDX analysis.
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Here, I mean the accuracy and the major differences.
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For otolith, you will probably want to analyse variation of some trace elements (ie. Sr, Ba), which appear to be non-detected or qualitatively detected by EDS ( ). On the other hand, ICPMS will provide your more accurate and consistent results for those elements. Remember that such technique give values for the whole sample, not particular region.
As stated by Esteban, LA-ICPMS stay the gold standard in otolith chemistry analyses, especially for its precise sampling of otolith material (by laser ablation), that provide accurate quantification of trace element in a given region (laser ablation radius is generally around 5-10 um). Hence, you could analyse fine variation along the growth axis, looking for fish ecology, migration or origin.
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I prepared an activated carbon by chemical activation process using H3PO4 as activating agent, the pHpzc of this carbon is 6, I analyzed this carbon by elemental analysis and by TPD to know its composition. I had different results on oxygen contents
For TPD the oxygen content is around 11.5 %
For elemental analysis the oxygen content is around 36 %
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Mohammed-El Amine Benchaabane Please, could you explain more your opinion specially about thermogravimetric analysis (TGA)?
In fact I did it for my carbon and the TGA curve presented a weight loss (~30 %) from room temperature until 900 °C.
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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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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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I recently submitted my samples to a laboratory for ICPOES, I am only provided with Standard Deviation and Mean data of one element out of two. I want to know if there is any spectra that is generated during the process?
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There will be data for as many elements as were calibrated. But you need associated QC if you are to rely on the data.
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Hi everyone,
i would like to extract some elements and molecule from soil for an Continuous-Flow Analysis (Futura, AMS Alliance) but for these analysis I only have very little material (about 0.1g). It is dust from the Sahel as part of a project on erosion. I want to analyze PO4 (Olsen extraction method and colouring of a phosphomolybdic complex ), NH4 (2M KCl extraction, Salicylate method on CFA), total phosphorus (HCl method) and NO3/NO2 (2M KCl method, cadmium reduction method). For quantification Do you think I can do these analysis with so little material? I’m open to advice.
Thank you so much
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sample is very small to carry out all these analyzes
best regards
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for my bachelor project I did some measurements on solid polymeric samples with an handheld XRF (X-MET8000 optimum). data of 13 different samples where collected, the data contained information about the measured concentration and 95% confidence interval. (see file)
I am not sure which validation/statistics/… method i can use to make a discission out of these results. i was thinking about an analysis of the average but then i do not know what to do with the 95% B.I.
it would be wonderful if anyone could help me with finding an appropriate method to process these results
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I often have troubles obtaining adequate elemental analysis for iridium compounds when the ligand is triflate (CF3SO3), hydrogen and nitrogen work well but carbon is usually about 5% lower and sulfur values are random, even in samples from the same batch. Does anyone know if this is frequent? Are there any references to problems in the analysis when there is sulfur in the organometallic samples?
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P.S. Don't tell you boss that I suggested to you to skip the sulfur values... 😂
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Hi i am working with PSI(pipe soil interaction) elements in abaqus. i am getting an error message as "The elements have been identified in element set ErrElemMissingSection. " i have included pipe-soil keyword in the keyword editor also. what should i do?
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Please look at the following below attached file which may help you in your issue.
Thanks
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I have to work with Aluminium foil (8079alloy- 38 micrometer thickness) , in the last months we encountered an adhesion problem between the aluminium and the coating materials (primer), so I think the problem is that the foil has some traces of rolling oil or other slipping addition from the source of the aluminium ! but how to make a test to be sure about this hypothesis .. I have a simple laboratory with no elemental analysis instruments.
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First, etch the Al foil surface with suitable solutions.
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We are developing a general method for Q3D elements by ICP-MS, out of all Q3D elements Au shows inconsistency in spike recoveries and bracketing standard recoveries. We are using 2% Nitric acid and 0.5% HCl in water(Trace elemental grade) as diluent. Au was analysed against Y and Tb as internal standards, results remain same. Some times we were getting recoveries with in limit (70% to 150%) with the same conditions the other time recoveries fell short. The reason for this is Au is not stable in HNO3 and HCl? or is there any other reason? and what would be the optimal conditions to get consistent results? (We are not using any glassware for sample preparation, we only use Poly propylene tubes throughout the analysis.)
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Thank you Hurst and Virgilio for your suggestion, i have tried with 5% HCl with 2% Nitric acid now the recoveries consistent withn in limits.
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the sample is a mixture of activated sludge with agricultural residues that have been subjected to anaerobic digestion for 40 days in order to biomethane production.
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Is your activated sludge wet or dry? Having said that, even air-dry materials can have a fair proportion of moisture that can alter your results, so drying at low temperature (60-80degC) for 24-48 h might be beneficial for between experiment consistency. If it is wet, then drying might lose a lot of volatile nitrogen compounds which may or may not be part of your analytical interests. (I assume you are not as interested in the fertilizer as much as the residues as nitric acid digests will add plenty of N to your sample).
There are many recipes for digestion procedures out there, but fertilizers might be need particular care as they are relatively concentrated and might react explosively compared to "typical" plant or soil digests.
Clear colourless digest is not as important as completely digested for your purposes: eg silicates will not normally dissolve unless using HF acid which requires specialized fume cupboards and full safety plans in case of spills. If you don't need to analyse for it, don't try to do a complete digest; filter out the lumpy bits and go ahead with the yellowish liquid most digests end up as.
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For the determination of percentage of limestone in Portland limestone cement using X-ray fluorescence spectrometer. By using the elemental analysis of major oxides is it possible to calculate this percentage ?
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CO2 from limestone (or other carbonates) is included in the loss on ignition, which is usually performed before XRF. However, LOI contains also bound water, e.g. from gypsum or hemihydrate. From XRF alone, determination of limestone is not possible.
You can do a thermogravimetric analysis to quantify CO2. CO2 can also be determined by combustion analysis or by a volumetric method measuring the volume of CO2 released when HCl is added to the cement. The limestone content can then be calculated from the amount of CO2, assuming that dolomite (or other carbonates) is absent, which is often not the case. Calcite can of cause be determined directly by quantitative X-ray diffraction (Rietveld analysis).
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I want to know if it is possible to make any definitive conclusion about Carbon present in Aluminium alloy from the EDS report as it might be highly inaccurate.
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Wrong. Carbon tape is a secondary source of C contamination, not really important one.
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Typically, several factors are considered, when deciding between Finite Element [FE] Analysis and Boundary Element [BE] Analysis, for a specific problem, and include whether the problem to be solved is a "Shell-type" Structure, "Linear" or "Nonlinear" application. It also depends on the degree of accuracy that you want to achieve, and the amount of time that will be necessary to prepare and analyze (interpret) the output data that will be obtained.
Keeping this in mind, what do you prefer to use for your Analysis work and Research ?
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Hi both of them has their own properties but in our country most of the engineers and researches use finite element method bcz it has been used in mostf of the softwarss and even has been studied more about it.
For example 3 friends of mine in our university are working on subjects that should be used by FEM. But it depends on the subject that you want to study and your guides opinion.
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We have some O-rings made of perfluoroelastomer (FFKM) from a different vendors and we would like to determine the cross-linking density to correlate with performance. Can anyone suggest a suitable technique?
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Sure... The segmental molecular weight (Mc) of a crosslinked polymer is conneted to its shear or elastic modulus. In principle, if you can evaluate G' or E' in the rubbery plateau, then the Mc value can be calculated following the formulae:
1) G' = dRT/Mc; and 2) E' = G'/[2(1+nu)], where G' is the shear modulus, E' the elastic modulus, d is the density of your material, R is the gas constant, T is temperature and nu is the poisson ratio.
You will not obtain a a value for the corsslinking density, but an averaged molecular weight between crosslinked segments. Please, remember: when highly crosslinked, smaller Mc values and higher G' and E' values...
SALUT!
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I was run 100ns MD simulation for native and mutant structures. Although, RMSD, RMSF plotting was done but I want to compare native and mutant structures through secondary structure element analysis. How can I start for building SSE plot from YASARA trajectory files?
Thanks in advance.
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You can use gmx dssp command in gromacs to analysis the secondary structure.
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while performing edx on powder MgB2 sample in TEM, i observe Cu and C intense peaks. I was thinking this might be because of the TEM grid i am using. But can anyone help me how to avoid these signals.
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Of course you cannot " choose the elements you expect in your sample to be detected", you'll detect everything (comments above are wrong). If you use carbon or polymer support film, you cannot get rid of C peak. You can decrease/eliminate Cu peak generated by a grid:
- Remove objective aperture during EDS analysis.
- Use top hat aperture
- Use Be (instead of Cu) grid, but it is rather expensive.
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Please I need information on laboratory that can undertake xrd (quantitative and qualitative) and elemental analysis using ICP-MS
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XRD and ICP-MS instrumentals are very common. Such Lab facility available in most of the countries.
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For the work on a project, I need to convert results from proximate analysis of wood biomass to elemental. After looking in the literature, I have found only Gebhardt formula applicable to coal. Is there any published method/formula to convert proximate analysis to elemental for biomass?
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Your point is valid Bemgba B. Nyakuma for lab analysis of fuel.
I asked for this correlation, because I am trying to make the conversion (proximate-elemental), for a sensor installed on-site in power plant, and I have a simulation model which requires elemental composition, to calculate the required parameters.
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I am searching possibilities of analyzing coordination sphere geometry of particular d-block metals contained in microcrystals (areas of up to, say, 20x20 microns) of a mineral embedded in a typical geological (electron-microprobe-dedicated) thin section. I was wondering if such an analysis is possible and if there is any laboratory that provides such analytical capabilities. The extraction of the mineral domains from the thin section using FIB is rather impossible in this case. I would be grateful for any suggestions of a laboratory where the above might be achieved. I am interested in the NMR analysis of H, Mg, Al, Si, V, Fe, Co, Ni, Ge and possibly Ag.
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Dear Scholars,
I need to know is there any possible lab, institute or organisation in world providing economical ICP-MS/OES based elemental analysis of soil and plant samples.
I need to get my samples analysed for Ce (III,IV) , if there is any such lab which can offer Ce analysis at economical rates (~2-3$) then i can ship my samples (100+) to sourced laboratory.
Need your kind response in this regard.
Thanks!
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Umair Riaz thanks
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Alright, I am trying to find LHV for a liquid fuel. Let's say the fuel is a type of gasoline. The first thing that came up to my mind was to perform elemental analysis, then calculate HHV using Dulong and Petit equation, then convert to LHV using this equation:
LHV = HHV – 2400 ( M+9H2) kJ/Kg
I know EDS is not an option, I also doubt whether GC-MS might be helpful.
I don't really know any other liquid fuel elemental analysis instruments. If someone's willing to share an insight, I'd be very grateful.
Thanks in advance
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To determine H content you need to perform a HCNS analysis (by elementary analyzer) or H-NMR.
Regards
G
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A strange fact has been noticed in an ICP-MS instrument equipped with triple quadrupole: After the performance check (interface check), the uranium (238 isotope) counts have been consistently lower than the counts for the In (115 isotope).
Theoretically, it is expected that the larger the element mass, the higher counts recorded by the detector. And this theory proves true in practice for all the other elements present in the TUNE solution. Only uranium contravenes the trend and presents lower counts (U <In).
Could any ICP-MS expert suggest a procedure to improve this performance? Anyone else with similar problem?
Relevant informations:
1 * Commercial tune solution: 1 ppb for each element
2 * Fact repeats with aqueous standards for different concentrations
3 * Formation of oxide <2% (measured by the ratio 140Ce.160O / 140Ce)
4 * Uranium oxide formation <3% (measured by 238U.160 / 238U)
5 * The U-signal measured in the TUNE solution is often below 330,000 cps (value set by the performance) and usually its stability is above 2%. After cleaning the sampling cone, the skimmer and the lens, an improvement in the Uranium signal can be immediately noticed. However, this signal remains less than that of the Indium (In) and after a short time of use (typically 1-2 hours) the U signal drops again and the stability worsens.
6 * Skimmer, torch and new cones have been tested and the situation persists.
7 * Situation continues, even after new tuning, mass and detector calibration.
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Dear Rodrigo Papai
I am not sure, where your "theory" originates from but as such it is not true that higher mass/charge isotope needs to have a higher sensitivity.
In fact, if you consider that a solution having the same mass concentration (e.g. ug/L) of U with atomic mass of 238 and In with atomic mass of 115 contains more than twice as many In atoms would contratict such a general statement.
As a second fact, quadrupole-based ICPMS usually operate in a way that mass resolving power is increased with mass/charge (leading to similar peak width across the mass/charge range), which theoretically would also favor lower mass/charge sensitivities.
It is a fact that sensitivity in ICPMS generally increases with mass/charge if the heaver ion has similar ionization energy. A significant factor is the so-called space charge effect, which attenuates stronger the transmission lighter ions. A second factor is higher mobility of the lighter ions in the ICP and vacuum interface, causing greater loss by diffusion. The actual sensitivities however depend on a large number of factors like ion optics settings, ICP operating conditions etc. Your data seem to indicata a substantial preferences for lower mass/charge isotopes (Li is twice the limit value) so probably your instrument settings are just not comparable to those used in your "theory".
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I did CHNS analysis of my biochar samples ans i have to g=find out these ratio. In some papers i saw they directly calculate it by the %C, %H, %N obtained by CHNS. but in some papers they minus the %ash content from %C content. and for some papers they did it with some entirely different way which i am not able to figure out. Kindly help me to figure out the right way to calculate these ratios.
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Sorry for late answer. That right ash content should not be avoided and molar ratios should be calculated like say if value of carbon content is 67% then its should be divided with atomic weight of carbon which is 12. In similar way for N, H and O all the % calculated values should be divided with their respective atomic weight and then with theses calculated values ratios should be calculated.
Regards
Amita
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I have to done use SEM-EDX for the imaging and elemental analysis of a fabric coated with metal nanoparticles. Do i have to sputter coat the fabric with is coated with nps ? Can i take the SEM images without sputter coating? I want to know, will i get dark image of fabric with illuminated nps on it. If yes then its fine if no then i want to know is the fabric visible? And if the gold sputter coating will have any reaction with coated nanoparticles which could alter edx data/result .. Suggest please.
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Hello Savy Panamkuttiyiel Minal,
The raised topic is interesting. In order to have better visibility, it is necessary to apply a coating with metal nano particles. Most often, the metal coating is made of gold due to its good conductivity and does not react with the biomaterials. Problem remains the size of particles that can change surface roughness because they are not the same size. may even block some openings. That's why the share of metal particles could be best. for analysis. This joints in special conditions with pre-fitted vacuum installations.
Wishing for success in scientific work.
Regards Emil Yankov
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It is a known fact that the Si/Al ratio of the cementitious matrix influences the behavior of the geopolymer concrete.
However, I would like to know about the effect of the Si/Al ratio of the cementitious matrix on the behavior/characteristics of a normal Portland cement concrete or high performance concrete made with supplementary cementitious materials.
-Also, is there any method to calculate the 'Si/Al ratio of the C-S-H' from the 'Si/Al ratio of the hardened concrete'?
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If I am understanding your question correctly, then the question doesn't really have an answer. In geopolymer concrete, Si and Al oxides are extensively linked and therefore the Si/Al ratio has a significance in terms of the polymer structure. But in OPC products, the primary structural backbone is C-S-H, wherein SiO2 is the primary counter-cation to CaO and only a small fraction of Si sites are Al-substituted. Other phases not found in geopolymer concrete, notably ettringite and monosulphate, contain a large fraction of the Al.
In OPC chemistry, the Si/Al ratio reflects the ratio of alite and (to a lesser extent) belite to tricalcium aluminate and calcium aluminoferite. Since the alite and (to a lesser extent) belite are the binding phases that are primarily responsible for forming C-S-H and giving OPC products their mechanical and durability properties, increasing the Si/Al ratio will improve all important properties of the OPC. From a perspective of concrete properties, there is no drawback to increasing the Si/Al ratio and, in fact, an "optimal" OPC would have Al content of zero. However, it is not possible to manufacture such OPC for a number of reasons (e.g., raw material availability and the need to form liquid phases of C3A and C4AF in the cement kiln).
Hope this helps!
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In so many publications, ICP-OES (inductively coupled plasma optical emission spectrometry) has been used for the calculation of nanoparticles concentration. Is it the right way? I feel that ICP-OES can do elemental analysis. Expecting your views.
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Dear Agnishwar Girigoswami
That depends a lot on the samples. If the size- (or rather mass-) distribution of metallic particles is well known and there is no significant contribution from dissolved metals of the same type in solution you can estimate the number concentration from the mass concentration of the element(s) determined in the suspension or digestion of the NPs. I would assume that determining the accurate mass distribution is the major challenge for most NP samples/suspensions, because most methods determine a (hydrodynamic) diameter, which is then used to calculate the volume and mass by assuming a sphere. Differences in NP shapes (and/or composition) will thus lead to additional uncertainty in the mass distribution.
You may check the publications for technical details on how the number concentrations were derived. I agree that many publications do not seem to realize how important it is to supply these data.
As opposed to what has been mentioned previously though, particles < 100 nm diameter will usually not differ substantially in their response in ICPOES (or even in ICPMS) when compared to dissolved ions. Using ions in solutions will thus allow for an adequate calibration for such metal-NP suspensions too.
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I have some data in which a number of the analyte concentrations (data points) obtained were below the quantitation limit (LOQ) of the method used. This is possibly as a result of both the low values of the analytes of intrest expected in the test samples and the method and instrument detection limits. In such a case, how are these "missing" data points treated during statistical analysis and subsequent interpretation and representation?
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There are numbers of way to solve the problem of values below detection limits, I list some of them:
1- Substitute LOD/2 for all of them.
2- If you want to use the substitution, it is better to substitute LOD/sqrt(2) (to consider for the variance as well).
3- Impute the values below detection limits using multiple imputation.
4- More advance statistical approach is to use the mixture model. A binomial model for below detection limit and a log-normal model for above detection model data.
Hope it helps.
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We are testing for surface elemental contamination in Plasma Sprayed Yttrium Oxide. The problem we are having is that our extraction solution is not beading up on the surface very well. Is there anyone that has experience doing this that can tell me the best way to prep the surface? The Yttria is sprayed on a small Aluminum coupon, and we need the extraction solution to bead up as much as possible. Right now we are having a lot of instances where our solution spreads across most of the coupon, which makes recovering the solution for analysis difficult. We also want to have more control over the extraction area.
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Assuming that the alloy is completely dissolved using acid digestion.
If possible, can someone please suggest the type of ICP to use?
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You can use radial view in ICP-OES
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We want to do the elemental analysis on sand samples with ICP-OES can anyone recommend a certified reference material which we could purchase?
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Thank you for information, will check these databases! Well, at this stage, the main focus is on Zn, Cu, Pb, Cd, Cr, Mn and macro-elements.
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I am looking for sample preparation technique for trace elemental analysis of spinel. I need to perform analysis using solution-ICP-MS. My colleagues advise me to put spinel sample and hydrochloric acid (or aqua-regia) into glass vessel, solder up the vessel and keep it in the furnace for 7~30 days at 250°C. The same method I see in old handbooks. In modern publications usually mentioned LA-ICP-MS, but I have no such device. Can I dissolve spinel in some acid (or mixture) using Microwave Digestion Workstation with PTFE or TFM vessel? Have somebody had such experience?
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Hi Maria Isabel Varas , here a reference that could help you to do that, But if you need other advice message me and I will send you the protocol we used in our department for low trace elements concentration it usually work for Spinel dissolution. You could also use the Alkali Fusion method with acid digestion (AFAD) method of Senda et al. (2014).
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I am trying to analyze Lead in water samples using an atomic absorption analyzer. I tried without modifier but i get really low absorbance levels. I guess I need appropriate matrix modifier to increase the signal.
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Note with using matrix modifier the furnace temperature program must be changed ashing and atomization temperatures must be increased
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Hello, I am currently researching a spectral computed tomography system for medical applications. The system excels in delineating the elemental composition of materials, providing a 3D representation of the each element's distribution. This has shown excellent results in determining the composition of calcifications but I'm wondering what other diseases researchers are aware of that might benefit from this technique.
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The elements that would be involved in examples I mentioned would copper, Iron and the compound silica.
Do you think this method could work in some of these cases?
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Cedar is the common name for cedar wood, used for several different trees that grow in different parts of the world.
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Please look at the following below links which may help you in your analysis:
Thanks
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The characterization along with chemical analysis of the adsorbent is essential for my study to know about the percentage of different chemical constituents in the adsorbent.
Please, suggest me the specific tests for characterization as well as for elemental analysis of the adsorbent.
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XPS should serve your purpose with proper sample preparation.
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Which technique is most suitable for elemental analysis in the environmental analysis?
Instrumental neutron activation analysis INAA
Inductively coupled plasma mass spectrometer ICP-MS
X-ray fluorescence XPR
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Hello, all depends which exact elements are you interested to analyse and which accuracy you need.
Also remember ICP/MS is destructive.
Here some advantages of all equipments.
The strengths of INAA are:
a. Can analyze a large number of elements simultaneously
b. Very low detection limits for many eleme