Elemental Analysis

Elemental Analysis

  • Yafei Wang added an answer:
    Does grinding and polishing influence the detection of elements under EDX?

    EDX is used to determine the elements on sample surface, combined with the observation under SEM. For metals, they are usually grinded or polished before observation. However the preparation process such as grinding by abraisive paper will contaminate the specimen. Accordingly, unexpected elements from abraisive paper such as Si and C could be detected through EDX, which has a bad influence on the results.

    Yafei Wang · Xi'an Jiaotong University

    Hi Yuriy
    You have proposed a very good point in your answer about the inteference of the polishing materials and the elements we are interested in. In other words, choosing the right polishing materials may solve the problem, of course, when there is an option.

    Best regards

    Yafei Wang

  • Marcial Yam added an answer:
    How do I prepare serum samples for the simultaneous determination of heavy metals using AAS?

    Want to perform elemental analysis of blood serum samples but not getting an easy one step method for sample preparation. References provided will be highly appreciated.

    Marcial Yam · Centro de Investigación Científica de Yucatán

    Well I told you, that you need consult methods of digestion dry or wet depending of the extracción, if you use microwave you can use 0.5 g of sample dilued in 25 ml of nitic acid, so you can check any book of standart methods of analysis to ensure he right quantity of nitric acid 

  • Nur Farahiyah Mohammad added an answer:
    How can I calculate elemental weight percent from oxide weight percent given by XRF?

    Hi everyone..I'm running elemental analysis using XRF for carbonated hydroxypatite. I want to find the elemental value of Ca and P. As we know XRF give the analysis in the oxide such e.g CaO . How to obtained the Ca weight percent from the CaO given by the XRF?

    Nur Farahiyah Mohammad · University of Science Malaysia

    Thank you all for the sugesstions.

  • Rina Singh added an answer:
    What are the techniques / methods to identify metal oxides in a mixture?

    I am working on the catalysts that contain different metal oxides. I want to identify the metal oxides.

    Rina Singh · Indian Institute of Technology Delhi

    XPS and FTIR can be used to identify metal oxides.

  • Jinbo Fei added an answer:
    How can I find the type of oxides present and their percentage based on EDX elemental analysis of a surface?

    Element- Weight%- Atomic%

    C - 8.77- 22.56
    O - 15.60- 30.13
    Al - 6.70- 7.67
    Si - 2.18 -2.40
    P -  0.32- 0.32
    S -  0.41 -0.40
    Fe - 66.02- 36.53

    Jinbo Fei · Chinese Academy of Sciences

    Possibly, XPS is the better way to get the precise answer.

  • Vivek Kumar added an answer:
    What are the rules of measuring mass elements in composition?

    Hello everyone, 

    I want to find the percentage of each elements in my thin film, the composition in my thin film is a mix of Al-Cu-Fe. I know,  I can measuring by ICP-MS or XRF. but I have two question:

    1st: Is the percentage for each elements different before and after annealing (temperature is around 800'c) or not?

    2nd: Do you know another methods for measuring the percentages or volumes for each elements (the max error for my composition is less  than 0.1% )?

    Vivek Kumar · Indian Institute of Technology Roorkee

    can anyone provide me the protocol for ICP-MS to quantify the metalloprotein from given sample

  • Mushtaq Ahmad added an answer:
    How do you calculate the degree of sulfonation for polymers using CHNS analysis?

    Can anyone tell me what the formula is to calculate the degree of sulfonation for poly(bis phenoxy)phosphozene from CHNS analysis?

    Mushtaq Ahmad · Pakistan Atomic Energy Commission

    It should be total S in sample analysed. Unfortunately paper did not show any CHNS data. I think you can use Varoon Singh formula and compare results with articles formulae. I am attaching another paper in which CHNS data and % SO3H is given.

  • Julie Perreault added an answer:
    What is the best method for dissolving rocks for ICP-MS?

    Hey Friends

    I need a clear method to dissolve variable rocks to determine elements (main and rare) by ICP-MS  System. 

    could you help me to get this method in clear steps

    thank you very much 

    Julie Perreault · Institut national de la recherche scientifique

    By  grinding your rock, you can perform an alkaline fusion into lithium metaborate 98.5%/ lithium bromide 1.5% flux. We already use this technic on geological sample for rare element.

    0.1g of grind powder in 1g of flux. Perform the fusion into platinum crucible with a fluxer (Claisse Corp.) and recolt it into PFA  beaker with 100ml of acid. (10%HNO3/0.5%HCL)

    We dilute 60 times to reduce the salt into the ICP-MS.

  • Le Zhang added an answer:
    Can someone help me with trace element measurement by SIMS?

    Recently, I used Cameca 1280HR to measure trace elements in basaltic glasses. The accuracy of most elements were +/-1-30%. However, Lu, Hf, Ta and Th (the contents of these elements are about 0.5-5 ppm) had poor accuracy (about 50% or even worse). The peaks of 180Hf and 181Ta were not good and it seemed there were some interferences (maybe 164Dy16O and 165Ho16O). But I don't know how to correct these interferences. The peaks of 175Lu and 232Th were normal. The interferences may be exactly overlaping Lu and 232Th. Could someone give me some advice to improve the accuracy? Thank you very much.

    Le Zhang · Chinese Academy of Sciences

    Hi, Zou, thank you for your information.

  • Bendiba Guedouar added an answer:
    What can WDS-SEM provide in addition to elemental analysis that is available in EDS-SEM?

    EDS: Energy Dispersive Spectroscopy 

    WDS: Wavelength Dispersive Spectroscopy using SEM

    Bendiba Guedouar · Centre Algérien de Développement des Technologies Avancées

    - WDS is second flight especially if you have overlapping peak between Elements
    then in this case the WDS makes distiction
    - WDS is as precise as EDS

  • Yash Gupte added an answer:
    I’m planning to investigate Al and Si co-deposition in silicophytoliths. Can anyone send me information about this subject?

    I am especially interested on papers about elemental anlaysis of silicophytoliths

    Yash Gupte · Ramnarain Ruia College

    diatoms & scanning electron microscope with AAS, dats all u need

  • Simone Cagno added an answer:
    How reliable is energy dispersive X-ray spectroscopy (EDS) for elemental analysis of powder sample?

    Is EDS sufficient to confirm the elemental composition of powder samples (composite) or is it necessary to go for advanced techniques like X-ray fluorescence (XRF) or XPS.

    Simone Cagno · Belgian Nuclear Research Centre

    You could also think of using XRD to identify the mineral/crystalline phases present in your powder

  • Matthew Wheal added an answer:
    Can anyone recommend a standard reference material to use when measuring the total P and Ca in fish tissue using ICP?

    Our goal is to compare whole-body Ca:P ratios between juvenile suckers with deformed opercula and without the deformity and between fish from two Oregon Lakes. I would like to know if deformed opercula that is observed on juvenile suckers and not on other species in UKL is likely to be caused by an imbalance in Ca:P. I would also like to know if the reason that the deformity doesn't occur in Clear Lake is due to a difference in the whole-body Ca:P. 

    Summary of methods: 1) Grind fish in a stainless steel blender (done), 2) ash fish blended fish at 550 C for 16 h, 3) weigh ash, 4) digest ash with HCl and/or HNO3 , 5) dilute with DI water to concentrations within limitation of instrumentation, and 5) use ICP to measure Ca and P.

    I am having a hard time finding a standard reference material of measuring P in animal tissue. I know these measurements are done but no one reports what standards they used. I could use suggestions.  Thank you for your help. 

    Matthew Wheal · Flinders University

    LGC standards list 24 fish materials on their website.

  • Santosh Kumar added an answer:
    How should one treat data with <LOQ values during statistcal analysis?

    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?

    Santosh Kumar · Central Electronics Engineering Research Institute

    In Statistical Analysis, If the data is not in our desired way, We have to apply the data preprocessing techniques to form appropriate data.

    Apply different different  preprocessing methods and then analyse them. It will be a better approac and I think It will be very Helpful to You. 

  • Dmitriy Berillo added an answer:
    How can I quantify modified arginine-chitosan without the use of elemental analysis?

    FTIR data is clearly showing modification of polymer, but i need a method for determination of quantification of arginine without use of elemental analysis.. 

    Dmitriy Berillo · Lund University

    Hello,

    I think that the simplest way to estimate a number of arginine in the chitosan is pH metric or conductometric titration of the modified polymer. To be able to do this experiment you will need only pH meter or conductometer. This method works well for linear and even cross-linked polymers.

    Here is a related reference: Metal complexes of amphoteric cryogels based on allylamine and methacrylic acid https://scholar.google.com/scholar?hl=en&q=Metal+complexes+of+amphoteric+cryogels+based+on+allylamine+and+methacrylic+acid&btnG=&as_sdt=1%2C5&as_sdtp=

  • Muhammad Aslam Baig added an answer:
    Can we determine elemental analysis of a material by using femtosecond laser and attosecond lasers as we see in the case of LIBS?

    As we know LIBS is mainly used for the elemental analysis of a material. Is it possible to use femto-second and atto-second lasers? If it is possible then which is a suitable technique and why? Is there any papers related to the elemental analysis by femto-second and atto-second lasers technique? Please give the reference also. Thanks.

    Muhammad Aslam Baig · National Center for Physics, Quaid-i-Azam University, Islamabad

    Nano second and femto second lasers can be used for the LIBS analysis. However, femto second laser are advantageous where surface or craters being produced are used for further studies. The nano second laser are more user friendly and easy to run and maintain.  

    Aslam

  • Tarik Ömer Oğurtani added an answer:
    How do I identify and quantitatively determine the composition of phases present in a composite?

    I have a composite containing oxides of Ni, Zn and P along with their elemental forms. For example, the composite may have the phases Ni2O3+ZnO+P or Ni+ZnO+Zn+P+P2O5 etc. Although EDAX gives the elemental analysis, its very difficult to ascertain whether the %Oxygen obtained is associated with Ni, P or Zn.

    Tarik Ömer Oğurtani · Middle East Technical University

    The powder mixture would be best test sample for the XRD measurements, one can even obtained particle size distribution and the average particle size using fast-Fourier analysis of XRD data, which may be important in the characterization of the final product.

  • Harsh Yadav added an answer:
    Why elemental analysis is not possible with X ray diffraction?

    Why is it that only phase analysis is possible using XRD?

    Harsh Yadav · University of Delhi

    The intensity of the XRD is depend on the structure factor. If you are exactly calculate electron density form its structure factor then you are able to show the exact concern atom belongs the fixed electron density point. The above routine is more accurate in single crystal XRD than powder XRD.

  • Syed Khalid added an answer:
    Which is better technique to detect the presence of 0.2 to 1% Nitrogen in the sample- elemental analysis or EDX analysis?

    Either elemental analysis or EDX analysis is better for identification low percentage nitrogen element. To me no need of quantitative accuracy also. Exact information on either present or not is required.  

    Syed Khalid · Beijing Institute Of Technology

    XRF is the best technique to analyze your sample

  • Jan Gunneweg added an answer:
    What is non-destructive sampling in Cultural Heritage?
    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.
    Jan Gunneweg · Hebrew University of Jerusalem

    Andreas, yes you are right that stone can be analysed by using magnifying glasses and portable XRF. Splendid for stone that will not suffer very much by such analyses.

    But what if you do that on parchment or on a drawing? The magnifying glass is not providing the requested information, whereas XRF portable or stable will damage the objects. XRF measured secondary X-Rays that return from an item after having been bombarded by primary X-Rays and the latter--irrespective how large the bombarded area--is not and will not beneficial for the artefact. Whether science has to stop or continue to work with X-Rays or even Gamma-rays is another question.

    I am of the opinion that sometimes--when it is really needed--one must analyze by destructive sampling. Getting results by virtual sampling is as yet impossible, hence my first remark that the term non-destructive sampling is obsolete

  • Kaj Heydorn added an answer:
    Can one use CRM other than NIST standards in Neutron Activation Analysis? if he did, can this jeopardise the results?

    Some researchers insist on the presence of a NIST standards in each Neutron Activation Analysis, saying: “ Certified Reference Material GBW 0xxxx (for example) cannot be used as standard. It can be only used as Reference Material for the estimation of precision and accuracy of results”.

    Why? Is it really inevitable to use a NIST standards, if so what is the use in the IAEA standards - for example-?

    Kaj Heydorn

    NAA is for elemental analysis, and calibration is therefore best carried out using weighed amounts of pure elements from any reliable supplier of analytical reagents.

    For QC/QA it is recognized practice to demonstrate validity by analyzing a CRM with approximately the same composition as the samples you analyze. All these matters are clarified if you read ISO 17025 or any similar local standard used for accredtitation.

  • Nadeem Raza added an answer:
    Which state of Fe element has more conductance Fe+2 or Fe+3 ?

    Pls reply

    Nadeem Raza · Bahauddin Zakariya University

    Fe in three oxidation state will have 5 unpaired electron for conduction of electricity or heat.

  • Dirk Luetzenkirchen-Hecht added an answer:
    How can I use EDS for my thin films on several different substrates?

    I have Cu2ZnSnS4 films on soda lime glass and Silicium wafer. I choose Si wafer for correct measurement of elemental analysis. In EDS analysis how can I ignore (or remove) Si from spectrum? Is it reliable measurement for other metals' composition. Any other reliable and robust method will be appreciated (not XRF beacuse I have no XRF facility in our lab).

    Dirk Luetzenkirchen-Hecht · Bergische Universität Wuppertal

    I would like to mention that Si K-emission lines do not overlap with any other EDX-signal from Zn, Cu, Sn and S! So it should not be a problem to separate the different elemental contributions!

    All the best, Dirk

  • Ian J Slipper added an answer:
    Can anyone explain me the difference between x-ray mapping and EDS in SEM?

    Thanks in advance.

    Ian J Slipper · Greenwich University

    Another point to bear in mind when mapping is peak overlaps. It is very easy to misinterpret a simple X-ray element map. For example we have studied heavy mineral suites which contain zircon (ZrSiO4) and fluorapatite (Ca5(PO4)3F). But the La line for Zr is 2.042 keV and the Ka line for P is 2.012 keV. Any energy window created for P will overlap that of Zr.

    So the simple X-ray maps for P and Zr will appear identical and you will not be able to distinguish the zircon from the apatite from this alone. In these cases is in essential to perform spectral deconvolution at each pixel to remove peak overlaps in order to see the true elemental distribution.

    Other well known overlaps are Na Ka and Zn La, Al Ka and Br La, Si Ka and W Ma, S Ka and Mo La and Pb Ma, Ti Ka and Ba La. If your systems contain any of these combinations beware of simple X-ray maps.

  • Dhrubajyoti Gupta added an answer:
    What is the main differences between NORM elemental analysis by using XRF technique and EDX technique ?

    I performed my analysis by using both techniques, one of them is sufficient or not.

    Dhrubajyoti Gupta · Inha University

    To add to what @Duke says above:

    In XRF bulk major element is done using fused sample pellets (for minerals or rocks its Std practice). However you can also get minor and trace elemental concentrations using powdered pellets made with the help of binders or palletizing aids. So the heterogeneous composition of the sample can be checked by SEM-EDX while XRF will treat the sample as a homogeneous bulk....its almost what @Duke already stated above :)

  • Aseel B Al-Zubaidi added an answer:
    Are EDS and elemental analysis techniques should give the same results of % composition for the same compound?

    Are EDS and elemental analysis techniques should give the same results of % composition for the same compound?

    Also, for EDS when calculating atomic% for C, N and O of my sample  were 33.72%, -0.33%, 66.61%. What is mean of negative value ??

    Aseel B Al-Zubaidi · University of Technology, Iraq

    EDS is used for chemical identification of elements and their concentration. XRD is used to identify spatial arrangements of atoms in crystalline phases.

    In EDS, electrons knock out electrons from atoms, producing X-rays of characteristic wavelength. These X-Rays are then detected to identify the element from which they were produced. In XRD, X-rays of known wavelength are used to probe the structure of the material, using the lattice as a diffraction grating.

    To perform an EDS you need an electron source. For XRD you need an X-ray source.

    If you are looking for chemical composition, concentration gradients, or solute segregation, use EDS.

    If you are looking for phase distribution, lattice strain fields or stored defect content, use XRD.

  • Yijun Zhong added an answer:
    How do I evaluate the sulfur mass % in S-C material of a lithium-sulfur attery cathode?

    Which characterization is more precise in evaluating the Sulfur mass % in S-C material of a lithium-sulfur battery cathode? TGA or elemental analysis?

    Yijun Zhong · Nanjing Tech University

    Thanks so much for Dr. Claus's and Dr. Stephen's suggestions, but in what way can Elemental Sulfur and Elemental Carbon be dispersed and dissolved in solution?

  • Nauman Rahim Khan added an answer:
    Can anybody help with copper ibuprofen complex preparation?

    I prepared a copper ibuprofen complex according to published paper in U.S.A in 1981 and I found that the elemental analysis and IR are in agreement with that in the paper, but the UV absorbance measured by my self  is 700 nm while in paper it is 644 nm, so I am confused is my preparation is right or not.

    Nauman Rahim Khan · Gomal University

    Dear Youssef

    Are you sure you are following that paper protocol 100%???like instrument, instrument model, specifications, solutions, chemicals of same grade, same manufacturer bla bla bla....I am sure you are NOT following that 100%...then no need to worry. Wave length of a compound can vary while using different instrument, different grade chemicals etc.....so its doesn't matter, if you are sure what drug you are using...and secondly UV method of analysis allows +-20 nm variations in lambda max...

  • Javier Miranda added an answer:
    What is the most preferable technique for elemental analysis on aluminum impactor stages for aerosols?

    I have a Berner impactor with aluminum foil as a collection media. I want to know different methods of elemental analysis composition of aerosols.   

    Javier Miranda · Universidad Nacional Autónoma de México

    If you do not want to destroy your samples, XRF is most recommended, as well as Particle Induced X-ray Emission (PIXE). As explained by D. Gupta, corrections for the filter itself can be done. EPMA may not be very useful, because it focuses mostly on single particle analysis and often the electron beam penetration is smaller than particle size. This is not the case for XRF or PIXE.

    However, for PIXE it is much better to use polycarbonate filters.

    IC or ICP are destructive techniques. IC is limited to only a few ions.

About Elemental Analysis

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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