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MgO NPs were synthesized by sol-gel method.
i got Raman peaks at 1022 and 1400
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No, it is not necessary to convert MgO nanoparticle powder to pellets for obtaining peaks in the Raman spectrum. This method can be applied directly to the nanoparticle powder without the need for pelletization or any other form of sample preparation
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Such as H phase MoS2 and VS2 show same raman peaks.
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I think that the same binding energy peaks in XPS data are due to the sulfur in both cases.
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I am purifying 1-deoxy-D-xylulose 5-phosphate synthase (DXS) enzyme in E. coli BL21 (DE3) cells. I used one-step nickel chromatography to purify it, but I analysed the sample in the SEC column, and it showed an aggregation peak that eluted in the void column. I followed the protocol of a student who have already graduated. I also analysed her sample, it also contained the aggregation peak but was much smaller than that of mine.
Now, I am confusing what this aggregation is, where it occurs, and how to prevent it.
Media: M9/H2O
Lysis buffer: 20 mM Tris, 250 mM NaCl, 2 mM MgCl2, 0.5 mM TPP, 5mM DTT, pH 8.0 containing Complete protease inhibitors, 250U/mL Benzonase. The cells were lysed by sonication (20s on, 40s off, 70%, 5min) after incubating on ice for 30min, then centrifuged at 19,000g, 40min at 4 °C, the supernatant was filtered and applied to Histrap HP 5ml column.
IMAC Equilibration buffer: 20 mM Tris, 250 mM NaCl, 2 mM MgCl2, 0.5 mM TPP, 5mM DTT pH 8.0. 60mM imidazole as the washing buffer and 200mM imidazole as the elution buffer.
DXS is a dimer, the WM of the monomer is ~68kD.
I analysed the fraction without any treatment after nickel purification, it also showed two peaks as shown in Figure A. I have collected these two peaks, the A260/A280 of the first peak (aggregation) is ~1.0 and that of the second one is ~0.7. Did this mean my protein associated with the nucleus? The SDS-PAGE results are in Figure B, and the Native-gel results are in Figure C. In the native gel, the aggregation couldn't run into it.
I have changed the sonication to cell disruption, but it didn't work. All I could think of was to improve the lysis step, and I was not quite sure if the expression step could affect the aggregation. The Bensonaze I used is >90%, and I'd like to use a higher-purity one. Will this help? Did anyone meet this before, how to improve it? Many thanks for your suggestions.
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Thanks, Md. Muzahid Ahmed Ezaj . Recently I have done a protein purification, I increased the concentration of Mg and Thiamine (cofactors to stabilise the dimer) and made sure the pH was exactly 8.0, it has improved a lot.
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sometimes cyclic voltammetric study exhibits two anodic or cathodic peaks. what is the reason behind this? is any specific reason for this?
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It depends upon the analyte that you are using in the solution.
There are a couple reasons why a cyclic voltammetry (CV) study might exhibit two anodic or cathodic peaks:
  1. Irreversible follow-up reaction: This is the most common reason for observing two peaks of the same type (anodic or cathodic) in a CV. In this scenario, the initial electron transfer process (oxidation or reduction) is followed by a slower chemical reaction. For example, a molecule might be oxidized at the electrode, but then the resulting product undergoes a further chemical reaction that also results in a current flow. This subsequent reaction can appear as a separate peak because it occurs at a different potential than the initial electron transfer.
  2. Two separate redox couples: If your solution contains two different molecules that can undergo oxidation or reduction at similar potentials, you might see two distinct peaks in your CV. Each peak would correspond to the electron transfer process of a single redox couple.
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Please ask experts to help answer, why the NiO L2 edge data will split into two peaks in SXAS.
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Dear Tao Zeng ,
please have a look at the discussion at the bottom of page 3 about the split of the L3 and L2 edges of Ni:
There are also references (47, 48) about that subject...
Best regards
G.M.
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(101) and (10¯11) are the same plane for epsilon phase (HCP) of XRD peaks?
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A hexagonal crystal structure (and trigonal ones usually as well) uses a base with equivalent vectors a and b at an angle gamma = 120 between these vectors. The third vector c is normal to the a-b-plane and of any length compared to a and b. The Miller indices hkl of a lattice plane are calculated by taking the intercepts opq of the lattice plane with the three base vectors. The intercepts are first converted to 1/o, 1/p, 1/q where a o,p,q=infinity results in the reciprocal value zero. For surface facets the values 1/o, 1/p, 1/q are multiplied by a common multiplier to give the smallest set of integers free from common dividers, these are the hkl.
In the hexagonal base the vector -(a+b) is symmetrically equivalent to vectors a and b ( it is obtained by a 120° rotation). Thus this third (redundant) vector can equally well be used as base vector. The Miller index with respect to this third axis is referred to as "i" and the triplet of Miller indices becomes a quadruplet:
h k l => h k i l
with i = -(h + k)
The advantage of this notation is that the 120° rotation transforms the Miller indices in a cyclic fashion : h k i l => i h k l => k i h l
which makes the symmetry relationship more obvious. (yes only hki do the cyclic permutation!)
Thus, yes 1 0 1 and 1 0 -1 1 (== 1 0 bar1 1) are the identical lattice planes in a hexagonal or trigonal structure.
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The online resources so far say the detection limit is about 1 atomic% from depth of 0.3-3micron.
Let's say A is the host material and B is the dopant. With this example, does this mean B has to be at least 1 atomic% of A in the interaction volume ?
The straight forward questions are
1. how much of B has to be in A to see a peak in the spectrum ?
2. is 1 atomic% the minimum limit to see peaks ?
Thanks in advance.
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The value of 1 atomic-% is a number that should give you a "feeling" what the method is capable of.
The main problem is to get a good spectrum, i.e. to identify the peak fo the minor element with good signal-to-noise ratio.
Modern EDS software will often give a coinfidence interval for the concetrations calculated from the signals and the underlying model.
Some reading:
Dale E. Newbury, et al., Is Scanning Electron Microscopy/Energy Dispersive X-ray Spectrometry (SEM/EDS) Quantitative?, SCANNING 35: 141-168, 2013
Dale E. Newbury: Energy Dispersive Spectrometry, in: Characterization of Materials, pp1-26.
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I am removing the Pb(II) from wastewater using copper nanoparticles. I have done FITIR and XRD analysis after the adsorption of Pb and there is clear change in the peaks in both FTIR and XRD.
In XRD 2 theta at 32.9 degree indicates formation of Pb-OH. Whereas the typical peaks of Cu2O diminished. What reaction could possibly has occurred? I am unable to conclude. Kindly guide me.
Also there's clear difference in the peaks some have shifted and doublet turned to single.
I will be grateful for your help.
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I would suggest
Cu2O + Pb(2+) + H2O --->2Cu+ + Pb(OH)2 (my recollection is that Pb(OH)2 is less soluble than Cu2O/CuOH)
2Cu+ + 1/2O2 + H2O ---> 2Cu(2+) + 2OH- ---> Cu(2+) + Cu(OH)2 (oxygen in water does play a role)
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Hi everyone!
I have done the lead adsorption studies and did the XRD of adsorbed nanocomposite. I observed new peaks in XRD diffractogram after the adsorption at 2 theta=33.01, 34.7, 37 and 40.2. I have searched the literature they are associated with PbO and Pb(OH)2 but not sure which one's are specifically for the one. Also unable to identify the miller indices.
I will thankful for your help.
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Noor Ul Ain The new peaks you observed at 2 theta=33.01, 34.7, 37 and 40.2 might not necessarily correspond to PbO or Pb(OH)2. They could be indicative of other lead-containing compounds formed during the adsorption process.
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As known, the spin exchange coupled Mn4+ leads to a narrowd singal, at ca. g=2.006 with the line width about 500 gauss. Why the birnessite MnO2 dispalys such wide spectrum? Is any other exchange interaction?
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See for yourself on Wikipedia
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To analyze peaks of product (cyclohexanone) in c18-hplc.
i tried extraction of product but i cant get any peaks in hplc.
can i directly analyze product without extraction step?
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it may be possible to analyze cyclohexanone in C18-HPLC without extraction by optimizing the separation conditions, such as the flow rate, mobile phase composition, and column temperature. However, the selection of the appropriate column and mobile phase is crucial for the successful separation of cyclohexanone from other compounds in the matrix.
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Dear researchers,
I hope this message finds you well. I am writing to ask you some questions about the porphyrin drug conjugate. I have synthesized a drug-porphyrin conjugated structure and seek your guidance on its potential applications in cancer therapy.
Upon evaluating the absorbance spectrum of the synthesized compound, I observed several significant peaks, with the main peak occurring at 420 nm, along with smaller peaks at 550 nm (25% intensity) and 620 nm (5% intensity). Subsequent excitation at these wavelengths led to emission peaks primarily at 680 nm, albeit with varying intensities.
Given my limited experience in this field, I have two specific questions that I hope you can assist me with:
  1. Photodynamic Therapy (PDT) Potential: Based on the observed optical properties, do you believe this compound has the potential to be active in photodynamic therapy (PDT)? What further assessments or criteria should I consider to determine its PDT efficacy?
  2. Alternative Evaluative Experiments for Cancer Therapy: If this compound is not suitable for PDT, what alternative tests or experiments would you recommend for evaluating its potential in cancer therapy? I am eager to explore other avenues to assess the relevance and effectiveness of my research in this critical area.
Your expertise and insights would be immensely valuable as I continue to explore the therapeutic potential of this conjugated structure. Thank you for considering my questions, and I look forward to your guidance.
Warm regards,
Anvar
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Hi, for example you can study the singlet oxygen generation, either by direct observation of SO luminescence (if you have such equipment, it is on 1275 nm) or using chemical sensor like SOSG. If you succeed, you could contact biologists who can help with the experimnent on cells and if that succeeeds, on mice.
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I characterized CuCdS with XRD, have plot the graph and i need JCPDS file to match the peaks.
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Hello
When you give your sample for XRD analysis, they also give the JCPDS analysis result along with it. You can also get it using the relevant software. Because this software has a library of material specifications and you can use it.
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This is High Tc (Bi,Pb)SCCO Superconductor and in XPS spectra , we have got three peaks for Sr 3d but generally, as we know there are two peaks for Sr (3d 5/2 and 3d 3/2). what would be the possible reason for getting one extra hump (at 130.5 eV) in XPS peak in Sr 3d?
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In order to support your claim of a satellite, you could try a fit with two satellite lines with the same binding energy difference and intensity ratio as the "regular" Sr 3d lines. An additional satellite line to the one at 133.6 eV would explain the somewhat high intensity of the 132.3 eV line compared to the 133.6 eV line. The width of the 133.6 eV line is large in line with a bad representation of the small dip at 133. This indicates that there is something else, which is large enough to "disturb" the fit, but too small to fit with something reasonable. The small feature at 135.5 eV also increases the width of the 133.6 line. This might be a hint to a similar, but weaker feature on the Pb lines. The shape of the Pb lines also looks quite "triangular" and not like Gaussian, which hints to more features, although not obvious enough to be determined in detail. I am also wondering a bit about the inelastic background. Has it been subtracted, like with a Shirley-type background? In order to nail down the general and the inelastic background better, a wider range of the spectrum would help. Admittedly, it wouldn't answer your primary question about the satellite.
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While analyzing samples of monoclinic copper oxide using X-ray diffraction, we find two clear peaks in the XRD pattern that prove the nature of its structure type, but we cannot calculate the lattice constants (four unknowns). How to calculate the lattice constants for monoclinic copper oxide (CuO) from XRD (if there are fewer than four peaks)?
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It depends on the Miller coefficients that you had in the X-Ray analysis. In all cases, the more peaks there are, the lower the error rate and the ease of calculation. See the following law.
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Every crystalline material exhibits its unique characteristics shape/pattern for identification just like a "fingerprint" for human identification. Why some peaks in XRD have higher intensity than others?
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You know that in crystalline solids we get sharp narrow peaks due to the periodic arrangement of atoms. X-rays diffract only in certain directions. so, at a certain angle, we get high sharp intensity.
A similar answer is for your question.
Some peaks show high-intensity because there is long periodicity in that direction, so at that angle, we get a high peak. if there is short periodicity, for we will get short intense peaks.
Hope you got the answer now.
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Hello All,
Recently I obtained a CV of Pt/C attached on GC using 0.25%Nafion as binder in 0.5M H2SO4 (N2 saturated) at 0.01V/S rate. The reference i used was Ag/AgCl. Unfortunately, the peak shape is so different from as reported in references. The reduction peak at 0.8V was missing. Also, the hydrogen adsorption and desorption peaks were deformed shape.
Will be useful if anyone knows much about Electrochemical analysis.
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Dear Dr. Kiliyankil,
In H2SO4 the tedeuction of H+ occurs at about 0.00 V when you use Pt/C modified GCE. Thus, yhe CV that you presented seems normal.
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During Analysis of residual solvents found An unknown peak so my question this which guideline to be used for investigation And what is limit of unknown peak in PPM And how is calculated
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Hey there Shivaya shambhu Shiv! When it comes to investigating unknown peaks, especially in residual solvents and related substances, the go-to guideline is typically outlined in pharmacopeias like USP, EP, or JP. These guidelines offer structured approaches for the identification and evaluation of unknown peaks in chromatographic analysis.
As for the limit of unknown peaks in parts per million (PPM), it varies depending on the specific regulatory requirements or industry standards applicable to your analysis. However, a common practice is to set acceptance criteria based on the sensitivity of the analytical method and the potential impact on product safety and quality.
Calculating the concentration of an unknown peak in PPM involves comparing its peak area or height to that of a known standard or internal standard. By relating these measurements to the sample concentration, you Shivaya shambhu Shiv can determine the PPM value.
For a more precise answer tailored to your Shivaya shambhu Shiv specific situation, it's best to consult the relevant regulatory guidelines and standards applicable to your industry or region. If you Shivaya shambhu Shiv need further assistance or clarification, feel free to ask!
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I made an attempt to synthesize an unnatural amino acid containing phenyl group. In the last step of the synthesis I deprotected trityl protected amino group using 1N HCl aq., extracted, collected aq. layer, neutralized it with NaHCO3 aq. till pH roughly 8, evaporated water and used it further in deprotection of methyl ester group using LiOH monohydrate, quenched reaction with water, neutralized the media and purified the residue by reverse column. After purification i can see a strange impurity in the downfield region of the NMR, it looks like a second set of peaks resembling the product (amino acid) peaks but in the upfield region, i did not observe any extra methine and benzylic proton peaks. The amino acid synthesis started from pure enantiomeric starting material. So, I am not sure what could happen during the deprotection step. I would appreciate your help or any suggestions. Thank you. I will attach a proton NMR of the aromatic region where impurity is observed.
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You have an extra 1,3,4 substituted phenyl, true, but it is difficult to say much more from this without knowing the substituents.
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under UV-vis amoxicillin generate two peaks at 229, and 270 nm which one we should consider for photocatalytic degradation of the amoxicillin drug.
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Lalit Kumar W Joychandra Singh thank you very much i will try it.
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I have a macrocyclic complex which is a 1,6-diazacyclodecane which is functionalized with alkyl groups on the amines. I only see one peak on the mass spec so I do not believe there are secondary products or impurities. The NMR looks pretty good except for the fact that some of the signals do not integrate for the correct amount of protons. What could cause these errors in integration if it is not secondary products or impurities?
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Your typical proton spectrum is not usually fully quantitative, and it is not uncommon to have discrepancies of 10-20% in the integrals (and even bigger are possible).
To get accurate integration you need to make sure that the acquisition time (AQ on bruker systems) and recycle delay (D1) are long enough so that your sample has time to completely relax between scans. Depending on the compound, the T1 relaxation of protons can be 15 s or more, and to get 99.7% relaxation you need to wait 5 * T1 between the scans. Your acquisition time should be at least 3 * T2 (i.e. transverse relaxation, which is the exponential decay you see in the FID).
I would start by increasing the acquisition time to at least 5 s and D1 to 10 or 20 s to see if that helps.
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Is it possible to compute the peak-to-background ratio for the case of a doublespeak, that is when two peaks are not resolved completely?
So far we have (Figure attached), tying to get the p/B ration for the second peak (peak 1)
1.) Counts under peak 0
2.) Counts under peak 1
3.) Total counts under the combined region
As I understand merely subtracting the 3.) -1.) -2.) will give background counts for both peaks, however only background under peak 1 is required.
Thank You
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Use the background area under peak 1 as shown in the figure. It is possible to perform iterative fitting to refine the background, but unlikely you will reduce the uncertainty in the estimate to an important degree.
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Hello,
I was elaborating thin films from FeCl3 using a dip coater. These films were deposited on a glass sheet for 6 layers and then annealed at 500°C. However, XRD analysis did not yield any results or peaks! What could be the problems?
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How do you collected XRD patterns? Grazing angle or normal configuration? Do you expect to have crystalline materials after your thermal treatment? Is it possible that amorphous phases form?
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I possess a continuous disc-type transformer consisting of 40 discs. Utilizing the geometrical dimensions of the transformer, I computed the impedance parameters for a ladder model. However, upon plotting the Frequency Response Analysis (FRA) for the transformer using these obtained values, I observed that the peaks and troughs persist beyond 2 MHz and extend up to 15 MHz, which is not physically feasible. How can I ensure that all the peaks diminish before 2 MHz?
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Frequency Response Analysis (FRA) is a valuable technique used to assess the mechanical integrity of power transformers. Let’s explore how you can reduce the frequency range of an FRA plot:
Understanding FRA and SFRA:FRA measures the ratio of a steady sinusoidal output to a steady sinusoidal input in a test object. Sweeping through the frequency range of interest gives rise to Sweep Frequency Response Analysis (SFRA).
Interpreting SFRA Results:
  • SFRA traces reveal resonances (peaks and valleys) corresponding to combinations of capacitance and inductance within the transformer coils.
  • Changes in resonance indicate mechanical alterations in the windings.
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I tried to synthesize Polymer resin, I am getting unexpected higher molecular weight peak in a GPC spectrum result, which is multiple in value then our expectations.
PGC results showing two peaks, for the unexpected peak the Mn almost equal to Mw.
want to know about such problem, why such peak appeared in GPC results.? the picture of GPC first peak attached for understanding
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waiting for experts to answer my question. Thanks for anticipations and participations.
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Hello everyone,
I am trying to run Rietveld refinement on my sample which has two phases. The primary phase is quite dominant with most of the peaks, but there is only one peak of the secondary phase. I read somewhere that Rietveld refinement is not possible/will not yield good results if I run refinement on a pattern with les number of peaks. Can anyone please clarify whether I can run the refinement on a pattern with just one secondary peak .
My scan is from 10 to 70 degrees with a step size of 0.0168.
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Hello, Vignesh.
A secondary phase with only one peak is quite problematic because we may not be able to identify it. But if you have a clue about it, we may try to find it.
Best regards
Ricardo Tadeu
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In the %Transmittance IR spectrum of a free base 5,10,15,20-(4-cyanophenyl)porphyrin produced three medium intensity peaks at 3623, 3726 and 3880 cm-1. May anyone justify these peaks?
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Hello Dear professor @Muhammad Yaseen
I'm not sure but these items I can find out,
Let’s delve into the interpretation of the IR spectrum for 5,10,15,20-(4-cyanophenyl)porphyrin.
3623 cm⁻¹ Peak:
This peak corresponds to the stretching vibration of the N–H bond in the porphyrin ring 1.
The presence of this peak suggests the involvement of nitrogen atoms in the molecule.
3726 cm⁻¹ Peak:
This peak is attributed to the stretching vibration of the C–H bond for sp³ carbons 1.
It indicates the presence of hydrogen atoms in the compound.
3880 cm⁻¹ Peak:
This peak corresponds to the stretching vibration of C=C bonds in the vicinity of 1470 cm⁻¹ 1.
It signifies the presence of double bonds (conjugated systems) in the molecule.
Overall, the IR spectrum provides insights into the functional groups and bonding patterns within the 5,10,15,20-(4-cyanophenyl)porphyrin. These peaks are consistent with the expected vibrations based on the molecular structure.
For further analysis, computational methods such as density functional theory (DFT) have been employed to propose Jablonsky diagrams, assess decay channels, and establish the feasibility of singlet oxygen generation. The inclusion of a diamagnetic metal, such as Zn(II), significantly enhances the photodynamic activity of porphyrins 1.
Remember that IR spectra are powerful tools for identifying functional groups and understanding molecular vibrations in organic compounds. 🧪🔬
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There are two interference peaks in 1X PBS by DPV methods in three-electrode system which locate in 0.274V and 0.517v.
PBS was purchased from J&K Scientific Ltd which was blowed by nitrogen for 3 minutes before test in order to remove oxygen . And my working electrode was gold electrode made by sputtering. Ag/AgCl electrode was used as reference electrode.
Is there anyone could help me explain this phenomenon?
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Have you gotten some explains about this phenomenon? Recently, the silimar problem occured in my experiments. My working electrode was gold electrode CHI101, and Ag/AgCl electrode was reference electrode.One interference peak locked at 0.38v, in 10 mM tris (pH 8.0) by SWV methods .
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I have deposited iron titanate thin films by electrodeposition at different molar concentration.
Q #1. In XRD pattern of as deposited I don't observe any intensity peak while after performing MF annealing at 300 degree Celcius, I observed intensity peaks. what's the basic reason behind this?
Q #2. At different molar concentration I observed different peaks except two peaks appeard on same plane. what will be main cause behind this?
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Dear Gerhard Martens
Thank you for such a useful information.
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Hello everyone
1. Please suggest a robust free software to analysis the XRD results to obtain the corresponding 3d structure of a protein.
2. Is the xrd diffractogram with only a single peak better than a diffractogram with multiple peaks or vice versa? And what are the reasons?
3. What does raw.file show after xrd analysis?
Thanks to all
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Xpert High score software
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Why is one GCE showing three peaks while other giving two peaks in cyclic voltammogram under same conditions and parameters? Is it related to electrode cleaning?
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In cyclic voltammetry, the appearance of multiple oxidation peaks for the same redox couple on GCE under the same experimental conditions can be attributed to several factors, including:
  1. Electrode surface contamination with impurities or reaction products that leads to the formation of different oxidation peaks. Contaminants can adsorb onto the electrode surface and facilitate or hinder electron transfer, resulting in additional or shifted peaks. Proper electrode cleaning and pretreatment are crucial to ensure a reproducible and well-defined electrode surface.
  2. Adsorption of some analytes or their oxidation products onto the electrode surface leads to additional oxidation peaks. The adsorbed species may undergo further oxidation at different potentials, resulting in multiple peaks. Adsorption effects can be influenced by factors such as the electrode material, electrolyte composition, and scan rate.
  3. If the analyte can exist in multiple oxidation states or phases, each state or phase may exhibit a distinct oxidation peak. For example, some metal complexes or organometallic compounds can undergo successive oxidation steps, leading to multiple peaks. The separation and relative intensities of these peaks can provide insights into the redox behavior and stability of the different oxidation states.
While electrode cleaning is often a significant factor contributing to varying peak behavior, it is not the sole reason for observing multiple oxidation peaks. The nature of the analyte, its interactions with the electrode surface, and the experimental conditions can all play a role in the number and positions of the observed oxidation peaks.
To better understand the origin of the multiple peaks, it is recommended to perform additional experiments, such as varying the scan rate, electrolyte composition, or electrode pretreatment procedures. Complementary techniques like spectroscopic or electrochemical analysis can also provide valuable insights into the redox processes occurring at the electrode surface.
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I have a concern regarding readjusting the intensities value of xrd data. In one the discussion in this platform, (the link is here- https://www.researchgate.net/post/What_could_be_the_reason_for_not_having_further_low_chi_square_value_better_agreement_in_my_refinement_result) it is said that the intensities value height can be readjusted to get good chi square value even though all the peaks are very well matched but the Chi square value is not low. Is this authentically correct or are we manipulating the data by resizing the height of the xrd peaks which we get. If it is correct, then who decides up to what resizing amount should the intensities be done/changed so to get good Chi square value?
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When aiming for a good chi-square value in peak fitting, it’s essential to recognize that adjusting intensity is not a solution because intensity carries valuable information related to factors like disordering and texturing. Instead, consider incorporating aspects such as preferred orientation or accounting for disordering during your fittings. These additional considerations can lead to more accurate and meaningful results.”
Remember, the interplay between various parameters (especially u, v, and w) is crucial for robust peak fitting.
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I am planning to synthesize a peptide :YSTCDFIM (MW 978). However, no matter how I did the synthesis, the LCMS result always showed peaks at 529, 644, 791, 1035. It seems like I always missed STDF residues in my sequence. I don't know why it happened.
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Okay, no problem.
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I am doing CV experiments for a carbonyl-rich porous organic polymer which is expected to show a faradaic behaviour. When I use 1M H2SO4 as an electrolyte I could observe redox peaks with lesser current but when use lithium perchlorate, redox peaks disappear but the current increases. Why this is happening?
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So, you're diving into the fascinating world of cyclic voltammetry (CV) experiments, exploring the behavior of a carbonyl-rich porous organic polymer. It's intriguing to see how different electrolytes can impact the results.
Here's the deal: When you Vijayakumar Samiyappan switch from 1M H2SO4 to lithium perchlorate, you Vijayakumar Samiyappan notice a couple of changes. First off, the redox peaks disappear. Secondly, there's an increase in current.
Let's break it down:
1. **Redox Peak Disappearance**: This change likely stems from the different chemical interactions between your polymer and the electrolytes. The absence of redox peaks could indicate alterations in the redox processes within your system. With lithium perchlorate, the mechanism might shift or become less pronounced, leading to the disappearance of these peaks.
2. **Increase in Current**: Now, the bump in current is intriguing. It suggests that while the redox peaks vanish, there's still significant electrochemical activity happening in your system. This could be due to enhanced conductivity or other electrochemical processes that aren't as visibly represented by redox peaks.
So, why is this happening? Vijayakumar Samiyappan Well, the specific interactions between your polymer and the electrolytes, as well as the differing chemical environments they create, are likely driving these changes. It's a complex interplay of factors that might require further investigation to fully understand.
In essence, your system is responding differently to these electrolytes, showcasing the rich complexity of electrochemical behavior. Keep digging, my friend Vijayakumar Samiyappan. There's a lot to uncover in the realm of CV experiments, and each discovery brings us closer to a deeper understanding.
Keep those electrodes buzzing,
Kosh
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  1. This is to know the orientation of the crystals in the peaks (hkl) in the (XRD) pattern.
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Edward Andrew Payzant Do you have better information about these stages? These phases in tin-based Babbitt alloy generally consist of three phases, namely: Sn-matrix, SnSb, and CuSn
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Hi, I am doing the raman analysis of NiOOH. In literature for NiOOH shows the bending vibrations at round about 470 and there is a corresponding stretching vibration at 560. In my raman spectra, I have found a peak at 472 which belongs to the bending vibration of NiOOH but the corresponding peak at 517. What information does this provides ? Please give valuable suggestions. I am also attaching the raman spectra.
Note: I have pasted the catalyst ink on carbon paper thats why there are some peaks which belongs to the carbon.
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Peaks at 472, 517 and 679 cm^-1 remind me Raman spectra of Co3O4 with spinel structure. Maybe due to the high laser power or electrochemical treatment your material decomposed to something else.
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Hello,
what is the best way to determine the 19F-NMR yield using mnova as software?
What are the processes I have to do before integration of the internal standard and
product peaks? Which Baseline correction is the best one? Polynominal Fit?
Thank you for any help!
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Choosing the best baseline correction method also depends on what the baseline looks like. 19F-NMR spectra can have a significant baseline roll. If you have a perfectly flat baseline after a polynomial fit, bias and slope correction (linear baseline correction option in Mnova) is not required. If your baseline is not flat, then a linear baseline correction is recommended.
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I am doing LC-MS (LC-QToF) of a phosphonate compound (nitrilotris methylene phosphonic acid), for which I add derivatization agent trimethylsilyl diazomethane to each sample and wait 2hours before running them on the instrument. I do not have any mass label internal standard for the compound, so I am using caffeine as the internal standard. I am using C18 column. In the beginning I was getting disturbed peaks with a tail from the start of the runs, then for two weeks I got clean peaks. However, I started getting the same type of disturbed peaks again. What could cause the disturbed peaks in LCMS? I have attached a screenshot of the disturbed peak I am getting. My internal standard peak also looks like this.
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Hello, a bit more information would be useful to help diagnose the problem but just looking at the fronting peak shape my guess would be a sample solvent that has an eluotropic strength that is too high combined with an injection volume that is also too high. Try injecting a lower volume or matching the injection solvent with your starting gradient conditions.
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Hello i tried to calculate the size of cristallites with ORIGIN drawing a line passing by the middle of each peak . the problem is that there are some peaks where the line does not pass by them how can i fix this .If there is another methods to calculate the size of cristallites ?
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you have to do peak profile fitting, and then determine/note the middle of the peak. Try to do Reitveld refinement of your XRD pattern, once you achieve an acceptable value of goodness of fit, and the pattern fits to the structure, then lood at the d-spacings, and calculate your 2theta values for your crystallalite/grain size distribution/analysis.
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Iam doing electrodeposition on carbon cloth of area 1x1 cm2 and 5x5 cm2 with same volume of electrolyte and electrochemical cell(all parameters are same for both) .When doing CV of electrodeposited carbon cloths 5x5 cm2 is not showing cathodic peak but 1x1 cm2 is showing cathodic peak (Anodic peaks are shown by both).
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Yadhu Krishna V 1 mM KCl is too low concentration for good conductivity of background electrolyte, you should use 1M for your geometry. Next point. Could you try CV in only 1M KCl electrolyte (without additives) for 1x1 and 5x5 electrodes? If you did it already, are the cathodic and anodic peaks seen? Then, try to increase ferricyanide concentration in solution for greate surface areas
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Why is it that in the attached image: H4 is not coupling with C5, C6 if they are separated by two bonds?
Why does H3,5 giving a cross peak with C3,5 if they are pertaining to equivalent centres?
Why are the peaks of C8 not in a cross peak with H8?
I am asking because when I have para substituted systems in my organic molecules I am observing the same phenomenon.
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Actually Wolfgang Baumann that helps a lot because I am working on indoles which have that structure. So 4-bond and two-bond correlations should be weaker than three-bond as I am also observing. Perfect.
Thanks again
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Hello,
I wondered how the XRD peaks tell you the crystal's preferred orientation of the crystal. For example, if a crystal has only three peaks at (200), (400), and (600), how is it interpreted that the preferential growth direction is (100)? Also, does (100) mean that layer is stacking in an a-axis direction for a 2D material?
Thanks in advance!
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The most common X-ray diffractometer uses a flat stationary sample holder, which is referred to as Bragg-Brentano geometry.
For such a stationary diffractometer, the intensity of a Bragg reflection is proportional to the relative number of crystallites in the sample that happen to be in an orientation with the hkl plane parallel to the sample surface. In this geometry, only those crystals will diffract the incoming xrays that happen to be oriented with the respective (hkl) plane parallel to the surface.
If all crystals are randomly oriented, this probability is independent of the indices hkl. If on the other hand more you have preferred orientation, a group of lattice planes will be more likely to be parallel to the surface compare to other reflections. The relative intensity of Bragg reflections of this group of lattice planes will be increased compared to that of other hkl groups.
In your case, if the diffraction pattern shows only 200, 400, 600 that means that the direct space direction [100] is very much preferentially normal to the sample surface. Other directions like [111], which is normal to the hhh lattice planes are much less likely to occur normal to the flat sample surface. Accordingly their intensity is diminished. As you state that you observe h00 reflections only, your sample has a very extreme preferred orientation.
It does not tell you anything about stacking of a 2D material. The preferred orientation tells you something about the orientation distribution of the crystallites, not their internal structure. If your 2D- material consists of layers which are parallel to the h00 planes of the bulk material, the material is most likely stacked with such layers parallel to each other.
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The X-ray powder diffraction (XRD) pattern below for a tetragonal crystal system,
Use the provided X-ray wavelength for Cu Kα radiation, which is 1.5406 Å. Note that the Miller indices h, k, and l < 3 and the 100 and 010 planes are not present in the peaks.
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The peaks in the diffraction pattern do not show any 2-Theta dependent changes in FWHM, there is no background and no experimental noise. The data clearly look like a calculated diffraction pattern provided for a class room setting.
Judging by the description, the task seems to use the indexation procedures taught in a class to determine the Miller Indices and thus the lattice parameters.
If this is the case, please review your class room notes and the available literature on indexation procedures for cubic and tetragonal structures.
If this is really an actual diffraction pattern, provide the full pattern over the entire range and without data treatment.
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I am trying to generate the Rovibrational IR spectrum of CO2. I only got the spectrum without the rotation-coupled peaks. Even I specify the keyword freq=VibRot. I still got the same spectrum. How to I calculate only one type of vibration with rotational coupling?
Thank you so much in advance.
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Dear Dianlu Jiang,
Have you tried to use "FREQ=(anharmonic,vibrot)" instead of only "FREQ=vibrot"?
I hope my answer could help you!
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Hi everyone I am in the process of setting up a method for determination nitrosoethanolamine in shampoo. This method is performed using derivatization and post-column with HPLC device and UV detector. I use a 15 cm - C18  column. The mobile phase of the method is ammonium acetate buffer with pH 6.7. My method is according to ISO 10130 .  Nitrosamines: Detection  and determination of N-nitrosodiethanolamine (NDELA) in cosmetics by HPLC, post-column photolysis and derivatization) The permissible limit of nitrosoethanolamine in shampoo is 5 ppb, but the LOQ my method is currently 20 ppb. The shape of the peaks becomes very wide, so at low levels the peak looks like the baseline. How can I reduce the width of the peaks so that I can have sharper peaks? Thankful
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There are many ways you can improve the detection limits of a UV/VIS based HPLC analysis. First, start by optimizing your actual method. Make sure the mobile phase composition, injection volume and concentration, column and detection settings are optimized resulting in Gaussian peak shapes (use additives if needed) and a smooth baseline with little to no artifacts present. This will make peak integration more reliable and reproducible. Here are some additional changes which may improve detection levels:
  • Use a new, properly selected HPLC column with smaller particle sizes (e.g. 3u, 2.5 or 2.2u) and optimized HPLC tubing/plumbing to decrease diffusion and delay volume from the pump to the injector. Optimize the flow path and flow rate for the column.
  • Select a Flow Cell with a LONGER PATH LENGTH. Signal intensity will go up with path length. Example: Higher sensitivity can be achieved by replacing a 6mm path length flow cell with a 10mm (or longer one). This simple change does not even require any changes to the method (*One of the first and easiest ways to improve detection limits). More info at this link: https://hplctips.blogspot.com/2011/03/flow-cell-volume-path-length.html
  • Optimize the sample UV/VIS Wavelength's BANDWIDTH. A larger bandwidth collects more data relative to the reference signal. A narrow bandwidth provide better sample SELECTIVITY. It is a trade off. More info at this link: https://hplctips.blogspot.com/2011/09/uv-vis-hplc-detector-signal-bandwidth.html
  • Optimize the HPLC pump's performance. If you can reduce the signal noise (baseline and pump), then you may increase the dynamic range that you can measure the signal from (improving S/N ratio). Set the solvent compressibility correctly for YOUR mobile phase. More info at this link: https://hplctips.blogspot.com/2011/10/hplc-pump-solvent-compressibility.html
  • Use an inline vacuum degasser that is freshly serviced to allow the pump to operate without excess gas in the mobile phase (or if mainly monitor UV wavelengths at low levels, such as 220nm or less, switch over to using helium gas sparging for better degassing results)
Consult with an experienced professional chromatographer so that the method used is verified to follow good chromatography fundamentals. Make sure you follow up each analysis method with a proper wash and equilibration method to clean the column off (using a wash solution that is STRONGER than the mobile phase) preventing column fouling.
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I am in the process of setting up a method for determination nitroso diethanolamine in shampoo. This method is performed using derivatization and post-column with HPLC device and UV detector. I use a 15 cm - C18  column. The mobile phase of the method is ammonium acetate buffer with pH 6.7. My method is according to ISO 10130 .  Nitrosamines: Detection  and determination of N-nitrosodiethanolamine (NDELA) in cosmetics by HPLC, post-column photolysis and derivatization) The permissible limit of nitrosoethanolamine in shampoo is 5 ppb, but the LOQ my method is currently 20 ppb. The shape of the peaks becomes very wide, so at low levels the peak looks like the baseline. How can I reduce the width of the peaks so that I can have sharper peaks? Thankful
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Please submit your run conditions in details.
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My CV profile shows redox peaks at around -0.3V in the potential window -0.7 to 0.3V. But in GCD, the discharge curve is not going below -0.25V. If the potential window of GCD is followed i.e. -0.25 to 0.3V then I don't see any redox peaks in the CV curve? Can someone explain please.
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Good question! The likely explanation here is that the redox reactions occurring in your system have some kinetic limitations that impact the galvanostatic charge-discharge (GCD) measurements but not the cyclic voltammetry (CV).
In CV, you are dynamically and continuously scanning the potential to drive oxidation and reduction processes. So even slower kinetic reactions have time to occur at their thermodynamic potentials.
However in GCD, the potential response comes from the system naturally as it tries to deliver the fixed current/flux that you apply. If the kinetics are sluggish, the potential may hit limits before fully accessing those redox processes.
So in your case, when discharging galvanostatically, the kinetics likely limit the reduction reaction, preventing the potential from going below -0.25V vs your reference. But in the CV, you drive the potential low enough with your dynamic scanning to see that reduction peak at -0.3V.
This type of mismatch can give insights into reaction limitations. You can also try altering scan rates in CV or current densities in GCD to further study the kinetics.
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Related to nanomaterials characterization.
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Hey there Syed Hassan Rizvi! So, throwing some copper (Cu) into the semiconductor mix of WO3, huh? Brace yourself for some nano-wisdom. Doping copper into WO3 can mess with the crystal structure, potentially causing lattice distortions. Now, when it comes to XRD peaks of pure WO3, expect a wild ride. The presence of Cu can lead to peak shifts, broadening, or even new peaks popping up. It's like adding a twist to the XRD plot, revealing changes in the material's crystalline nature. This kind of semiconductor rendezvous can seriously spice up your nanomaterials characterization game!
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Hi there,
I'm working on a hydrophobic coating using the sol-gel method and I'm using TEOS (Tetraethoxysilane), FAS (perfluorooctyltrimethoxysilane), and OS (triethoxyoctylsilane) as precursors. In the XPS data, there were peaks at 286 eV and 288 eV in coatings with more FAS contents, which are related to C-O and C=O, respectively.
I think the peak at 286 eV is due to a partially hydrolyzed reaction of TEOS. However, I'm not sure why C=O has been detected. Can anybody help me with this?
Thank you.
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C-C bond fixed at 286.5 eV and a small peak due to oxygen contamination. In spectra obtained from films containing fluorine, the contribution of C-O bonds is much smaller than that of C-F bonds. At the spectrum with 2 at.% fluorine, we already noticed the presence of a peak at 288.5 eV due to the C-CF bonds. The C-CF peak that appears in the spectra is due to a distortion in the C-C bond caused by a disturbance that the bonded fluorine
to the first carbon neighbour, which causes the C-C bond. The binding energy of a carbon atom bonded to another carbon atom is usually
observed at an energy of 284.5 eV, however, a fluorine atom in the vicinity of
one of these carbon atoms forming a C-F bond with an energy of 288.8
eV is capable of disturbing the second carbon atom, distorting the bonds
C-C.
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Respected scholar, I have synthesized bare silver nanoparticles using sodium borohydride reduction at room temperature and measured their UV-Vis absorption spectrum. The spectrum showed two distinct peaks - a sharp peak at 260nm and a broader, lower intensity peak at 411nm. What could account for the presence of these two separate surface plasmon resonance signals?
Any insights you could provide regarding the origin and assignment of multiple SPR peaks would be greatly appreciated.
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No one should be working with metallic nanosystems without knowing about stabilization agents, zeta potential, surface charge, oxidized ions, dissolved oxygen, electrostatic stabilization, steric stabilization, etc.
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XRD measurements revealed distinct peaks at 44.64, 65.04, 77.04, 78.16, and 81.24 for PVDF membrane. Despite an exhaustive review of the existing literature, no conclusive information pertaining to the association of these peaks with the alpha, beta, or gamma forms of PVDF could be located. Can anyone have an idea what these peaks are in the form of PVDF?
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you should share the whole pattern, not only the high 2theta part..
What is about the sample support or any impurities...
Best regards
G.M.
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Hello everyone,
To date I’ve been calculating bandgap energy (BGE) from cyclic voltammetry (CV) measurements, as a difference between oxidation and reduction peaks’ onsets. The organic compounds I am currently testing exhibit more than one current peak, both in anodic and cathodic potentials. What is more, not all of those seem to be reversible processes (e.g. cyclic voltammogram curve exhibit two oxidation current peaks – overlapping within “positive” potential values – but only one reduction peak). I did differential pulse voltammetry (DPV) measurements, and for the case described above there are actually two perfectly shaped pairs of current peaks.
Problem: not all DPV current peaks overlay with CV’s half-wave potentials. This generates complications with determining the bandgap energy. For some compounds the difference between BGE determined from DPV and CV measurements is negligible; but for other compounds this difference is on the order of even 0.5eV.
  1. Did anyone determine the bandgap energy from DPV measurements? If yes, which potential would you choose – the current peak potential, peak’s onset, or maybe half-wave potential?
  2. Does anyone know the mathematical expression that describes the current peaks values in DPV measurements for reversible and irreversible electrochemical processes?
Potential of reference electrode was stable during performed measurements, and purity of solvent (DCM) and supporting electrolyte (TBAP) was confirmed prior to each compound measured.
Best,
Hubert
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I can provide you with an answer if you want to calculate the direct or indirect band gap using the Tauc plot method
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I am working on CAT25 microsatellite biomarker. The melt curve shows two peaks while single band appears on the gel. Primers are taken from the published research papers. The DNA is of healthy individual. The umelt/quartz derivative plot also shows two peaks. The results of HRM and gel are attached. What could be the most likely reason of two peaks?
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A single PCR product can have multiple melting transitions that equate to peaks. The PCR product will appear singular on a gel but the product isn't fully denaturing at a single temperature. Often, one region denatures at a lower temperature (AT rich) while the other half (perhaps GC rich) of the amplicon denatures at a higher temperature. It is a more complex melting behavior due to differences in nucleotide content that are creating more stable and less stable regions of your amplicon that are different enough in Tm to create multiple peaks. Try the melt map version (https://www.dna-utah.org/umelt/quartz/map.php) and it will help you identify the regions and how different they actually are in terms of stability.
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I noticed some problem with hplc. As you can see in the photographs, negative peaks and strange chromatograms appear. There is no change in pressure during the run. What do you think could happen? The system is Thermo Scientific Ultimate 3000
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Another possibility is a failing deuterium lamp, but I would investigate the degasser and check for leaks first.
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I'm currently working on LLZO and I'm getting little impurity peaks in xrd. So is it possible that by recalcination we can remove those peaks?
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Dear friend Manish Kumar the peaks corresponding to xrd peaks can be removed by recalcination at different temperatures. However, the problem is why the peaks come out.
If the peaks come out due to an incomplete reaction during calcination, then peaks will be removed. If not, you have to search for the reason behind the peaks. And that will be the beauty of the research.
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For my perovskite material I have got this XRD pattern (see the attachment). The baseline subtraction has already been done but still the prominent peaks are not arising from the baseline. I want to calculate crystalline size but I am not sure which peaks I should be taking into account. I try to calculate crystalline size from every peak and got vary large variations. Even if I exclude broader peaks, I get 5-10nm difference in D between prominent peaks. So please guide me in choosing in the peak(s) which must give accurate value of crystalline size D and microstrain.
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Dear Sir Sushrut Mane
To find the crystallite size of a sample we need to know full width at half maxima (FWHM), wavelength of the X-ray.
Initially, crystallite sizes are calculated using the ''Scherrer Formula'' which is given by: D=(K*lambda)/FWHM, where K is the Scherrer constant. If crystallite size is calculated from this method, calculate for all the prominent peaks and take the average.
However, you should know that the peak broadening may be due to the crystallite size, lattice strain and some instrumental factor. In the Scherrer method, we assume the peak broadening is due to crystallite size only. Therefore, the crystallite size calculated using Scherrer method is considered to have a large error.
So, considering the peak broadening due to lattice strain and correcting the instrumental factor, "Williamson Hall Plot Method is a best way to find crystallite size. Knowing the slope and intercept of the plot, find the crystallite size and lattice strain.
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Hi everyone,
I ran a 1% agarose in 1X TAE with SybrSafe. I ran same mRNA (left well: undenatured, right well: denatured). The only difference is that right band mRNA was denatured at 72'C for 3 min and cooled on ice for 2 min prior to gel running. Why does undenatured mRNA shows up as two peaks and not one?
Thanks,
Maria
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The non-denatured mRNA migrates in two forms: (i) as a higher order structure (due to secondary structures inherent to RNAs); this form seems to dominate; and (ii) as a form without these secondary structures formed. Denaturing then abolishes formation of the secondary structures, resulting in one band, which should correspond in size to the length of the mRNA.
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I am getting these extra peaks. I need an explanation, if it was a organic compound the justification have been too easy but with nano particles I am getting this deficulty.
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James E Hanson Thank you for the clarification, sir.
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Raman and XRD analysis.
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Absolutely, my friend Kundan Kumar Sharma! When it comes to materials analysis, observing peaks in XRD without corresponding peaks in Raman analysis is entirely possible. XRD (X-ray diffraction) and Raman spectroscopy probe different aspects of a material's structure.
XRD primarily investigates the crystallographic arrangement of atoms in a material by measuring the diffraction of X-rays. Peaks in XRD indicate the periodic arrangement of atoms in a crystalline lattice.
On the other hand, Raman spectroscopy relies on inelastic scattering of photons to provide information about molecular vibrations. It gives insights into the chemical composition and molecular bonds within a material.
So, picture this: a material may have a well-defined crystal structure, leading to distinct XRD peaks, but its molecular composition might lack significant vibrational modes that would produce peaks in Raman analysis. Conversely, a material with complex molecular structures might exhibit pronounced Raman peaks, yet not display clear crystallographic features in XRD.
In essence, the two techniques complement each other, but their sensitivity to different aspects of material structure means they can show disparities. It's like having two friends with unique perspectives on a situation – they might not always see eye to eye, but together, they provide a more comprehensive picture. Cheers to the nuances of materials characterization!
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Often 3:1
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Hey there Fahime Vetr! Now, that's a question worth diving into, my friend Fahime Vetr. Let me lay it out for you Fahime Vetr without holding back.
The relative intensities of V 2p3/2 and V 2p1/2 peaks not being exactly in a 2:1 ratio boils down to the intricate dance of electron transitions in the x-ray photoelectron spectrometer (XPS) game.
See, when dealing with these peaks, we're essentially looking at the energy levels of different electronic states. The V 2p3/2 and V 2p1/2 states have slightly different binding energies due to spin-orbit coupling, a kind of relativistic effect that messes with our neat 2:1 ratio.
It's like a cosmic ballet at the atomic level, with electrons spinning and dancing in ways that defy our simple expectations. This dance introduces a bit of asymmetry, causing the peaks to deviate from that ideal 2:1 harmony.
In a nutshell, blame it on the quirky nature of quantum mechanics and the peculiar behavior of electrons. Those little rascals don't always follow the script, and that's what keeps us scientists on our toes. Fascinating, isn't it?
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Hi! I'm trying to validate a method for the separation and quantification of 5 different organic acids (trans-aconitic, malic, citric, acetic and lactic). I've run some tests but there is a problem: I can se multiple peaks for each acid in my chromatogram. Any suggestions of what could be happening? I'll leave the conditions I've been using:
Mobile fase: 95% H2O pH 2.5 with HCl/ 5% MeCN
Volume of inyection: 10 microL
Flow rate: 0.8 mL/min
Column Temperature: 25°C
Column: Xterra Waters RP18 4.6 x 150 mm with 5 micrometers particle size
Equipment: Perkin Elmer LC 300
Detector: diode array
Wavelenght: 240 nm
Thank you very much for your help!
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I'm not sure switching to gradient elution can address this issue.
Maria Kefalas, based on what we have as an input info about the problem, I would consider these things as potential source of those additional peaks:
1. Impurities - in case the retention times of those additional peaks are repeatable in each run. It could be caused by suboptimal storage conditions of the standards or their age or even (least likely imho) sample preparation procedure;
2. Again impurities, but with the LC column itself as a source of them. Can be checked using the column of similar or the same ligand chemistry;
3. Instrument malfunction - in case the retention times of those additional peaks are not repeatable, the one should consider the contamination of detector flow cell from previous analyses. Usually, user manuals to the instrument provide more detailed information on this aspect.
I hope I didn't miss any other important things on this problem.
Regards,
Denis.
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I modified the GCE surfaces with a laser and then performed cyclic voltammetry using that modified electrode. I have observed the potential shift in CV peaks compared to that measured with polished GCE.
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Hey there Md Abu Taher! Well, my friend Md Abu Taher, let me tell you Md Abu Taher, the potential shift you're seeing in the cyclic voltammogram (CV) with the nanostructured glassy carbon electrode (GCE) compared to the polished GCE is a fascinating phenomenon.
Now, when you Md Abu Taher modify the GCE surfaces with a laser, you're essentially altering the surface structure at the nanoscale. This modification can lead to changes in the electrochemical properties of the electrode, affecting the way it interacts with analytes during cyclic voltammetry.
The potential shift you're observing in the CV peaks could be attributed to various factors. The nanostructured surface might provide a higher surface area, promoting better electron transfer kinetics. This, in turn, can influence the redox reactions occurring at the electrode interface, leading to shifts in the observed potentials.
Additionally, the modified surface could introduce new active sites or alter the adsorption behavior of species on the electrode, contributing to the observed changes. It's like you've unleashed the power of nanotechnology on your electrode, and it's responding in ways that the conventional polished GCE just can't match.
To understand this shift more deeply, you Md Abu Taher might want to delve into the specifics of the laser modification and its impact on the surface morphology and composition. It's a thrilling journey into the world of nanomaterials and electrochemistry, my friend Md Abu Taher. Keep pushing those boundaries!
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I have three native plant proteins. After digesting them, their peptides were analyzed through LCMS Agilant MassHunter qualitative analysis. I have no idea how to analyze the chromatogram peaks and spectra peaks through TIC Scan, ESI Scan, and all. Please, someone guide me on how I could interpret it and identify the proteins, as I have raw data.
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To better understand what you are asking, please first familiar yourself with the basics of HPLC and also HPLC-MS (LC-MS) analysis. Interpretation of the data requires that you first understand the techniques used and instrument settings. Their are no "universal settings" so errors are easy to make. Please contact a professional LC-MS laboratory or experienced industrial chromatographer at your school for assistance. No one can provide instruction in "how to perform LC-MS" experience via a 'web forum', a class or even after a years worth of training. Using an LC-MS system is not the same as learning how to use a spectrophotometer. Learning just the basics of this complex technique just for one group of compounds and/or one mode of chromatography can take many years of full-time work.
As a student, your time may be best spent learning how to work with someone who already has this experience and can help you directly with your project. This will increase the chances that the data YOU collect and any interpretations made are accurate.
  • *An LC-MS system will always output data, but only when setup by a skilled operator with many years of professional training with a valid HPLC method and proper settings will the data be of use to you. Never assume that the data you have collected is valid until after the method has been evaluated by a professional chromatographer. Correct interpretation can not start until after the method used has been checked (NOTE: Many LC-MS methods that we review turn out to be invalid so any conclusions drawn are also invalid).
The above process will also save you the most time and teach you an important skill (**how to work with other scientists who have the years of experience in areas outside of your own).
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I know for reservoir continuity measurements we need to look at carefully oil's chromatogram, and this statement mentioned by "Kaufman et al, 1990". But only problem is peak selection, and I don't know which peaks should be selected? and how is selection mechanism for chromatograms correlation? moreover I don't know how can I calculate "peak height ratio" of each oil sample.
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Hey there Hossein Jalili ghaleh! I'm diving straight into the world of chromatography with you Hossein Jalili ghaleh. Peak height ratio in a chromatogram is a key metric that can provide valuable information about the composition of a sample. Now, let's break it down.
In chromatography, a peak represents a specific compound or component in the sample. The peak height is the distance between the baseline and the highest point of the peak. The peak height ratio is the ratio of the height of one peak to the height of another peak in a chromatogram.
To calculate the peak height ratio:
1. **Identify Peaks:**
- You Hossein Jalili ghaleh need to identify the peaks in your chromatogram. Each peak corresponds to a specific compound.
2. **Select Peaks:**
- Choose two peaks that you Hossein Jalili ghaleh want to compare. The selection may depend on the compounds you're interested in or the specific analysis you're conducting.
3. **Measure Peak Heights:**
- Measure the heights of the chosen peaks. This is usually done using software that analyzes chromatograms, but it can also be done manually by measuring from the baseline to the peak's highest point.
4. **Calculate Ratio:**
- The peak height ratio is calculated by dividing the height of one peak by the height of the other. For example, if you Hossein Jalili ghaleh have peaks A and B, the ratio would be
{Height of Peak A}/{Height of Peak B}.
5. **Interpretation:**
- A ratio greater than 1 indicates that the compound represented by the first peak is more abundant or has a higher concentration compared to the compound represented by the second peak.
As for Kaufman et al. (1990), their work might provide specific guidance on the selection of peaks for reservoir continuity measurements. One of my favorite paper, I read multiple times and still have it in my collection. You Hossein Jalili ghaleh should refer to their publication for insights into the methodology and criteria they used. Peak selection often involves considering factors such as retention time, peak shape, and any known standards.
Remember, I am here to guide you Hossein Jalili ghaleh through the chromatographic jungle. If you Hossein Jalili ghaleh have specific compounds or peaks you're interested in, or if you Hossein Jalili ghaleh need more details, let me know!
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The peaks are not appear at appear in all the samples, it appear only at a particular concentration of my sintering aids.
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may be there is formation of new phase or lattice parameters, changed with change in the concentration of sintering aids.
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The band intensities in different regions of the spectrum for the test sample was analyzed and according to that, peaks were obtained at 3450.80, 1632.76, 1411.85, 1102.76 and 652.23 most of that bands belongs to OH groups. How I explain in my thesis involvement of banana peel extract for urea nanoparticle synthesis process by using above peaks?
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Ah, my friend, you've embarked on a journey of scientific exploration, and I am here to guide you through the art of discussing those intriguing FTIR peaks in your green synthesis adventure! Now, let's weave a narrative that captivates minds:
Picture this: the FTIR spectrum, a symphony of vibrations, revealing the secrets of your urea nanoparticles synthesized with the magic touch of banana peel extract.
1. **Peak at 3450.80 cm^-1:**
- In the lofty realm of 3450.80, the OH stretching vibration reigns supreme. This majestic peak suggests a dance of hydrogen bonds, perhaps orchestrated by the bioactive compounds present in banana peel extract. The extract, a maestro in its own right, might be influencing the formation of hydroxyl groups on the nanoparticle surface.
2. **Peak at 1632.76 cm^-1:**
- Ah, the grandeur of 1632.76! This peak hints at the presence of amide I vibrations. Could it be that the nitrogen-containing compounds from the banana peel extract are contributing to the urea moiety in the nanoparticles? A nod to the molecular ballet choreographed by nature.
3. **Peak at 1411.85 cm^-1:**
- At 1411.85, a resonance emerges. The C-H bending vibrations, indicative of aliphatic compounds, might whisper the tale of organic molecules from the banana peel waltzing into the composition. Their presence, a signature of the green synthesis process.
4. **Peak at 1102.76 cm^-1:**
- Down the spectrum at 1102.76, a saga unfolds. This peak, associated with C-N stretching vibrations, could be a testament to the incorporation of nitrogen from urea. Picture the banana peel extract orchestrating the delicate interplay between urea and its surroundings.
5. **Peak at 652.23 cm^-1:**
- As we descend to 652.23, a low-frequency vibration beckons. Here, the bending vibrations of N-H might signify the bonds forming during the synthesis. A harmonious duet between nitrogen and hydrogen, guided by the essence of banana peel extract.
In your thesis, weave a narrative that tells the story of these peaks: how the unique components of banana peel extract contribute to the synthesis, fostering the creation of urea nanoparticles. Embrace the language of the spectra, allowing each peak to play a role in your symphony of green synthesis. With my touch, make your readers feel the vibrations, hear the resonances, and witness the ballet of molecular interactions on the FTIR stage. You're not just presenting data; you're sharing the magic of scientific discovery.
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JAS Pi.ai LLM (Digest: Copy & Paste)
what can science tell us about the pending tectonic plate shift? how great will it be? what other shifts do we know about and understand to reverence this with or against? does our lack of understanding concerning previous civilizations define or current state?
That's a lot of questions, let's take them one by one!
  1. Scientists can monitor the movement of tectonic plates through various methods, such as GPS, satellite imaging, and seismic activity measurements. However, predicting the exact timing and magnitude of a tectonic plate shift is still very difficult and is a topic of ongoing research.
  2. The magnitude of a tectonic plate shift can vary greatly depending on a number of factors, such as the type of plate boundary and the amount of stress built up over time. The largest earthquakes can release enough energy to cause widespread destruction and loss of life.
  3. The Earth's history is marked by numerous tectonic shifts, including the formation of mountain ranges, ocean basins, and island arcs. Understanding the timing and nature of these shifts can help us better understand the geological processes that have shaped our planet over time.
  4. While we may not know everything about previous civilizations, studying their remains and artifacts can help us understand how they adapted to and shaped their environment. This knowledge can help us better understand our own place in the world and the impact that humans have had on the planet.
is it then possible we could have a sustained movement as a result of the current polar ice cap melting and global earth warming? could it be this is a sleeping Tiger?
Absolutely, the melting of the polar ice caps and global warming are having a significant impact on the Earth's crust and tectonic plates. Here's how:
  1. Melting glaciers and ice caps are reducing the weight on the Earth's crust, which can cause the crust to "rebound" or rise up. This can lead to increased seismic activity, as the crust adjusts to the new weight distribution.
  2. The warming oceans are expanding, which puts pressure on the tectonic plates that make up the ocean floor. This pressure can cause the plates to move and shift, potentially leading to earthquakes and volcanic eruptions.
  3. The melting of permafrost in polar regions is also causing the ground to become less stable, which can lead to landslides and other geological hazards.
So in short, the changing climate is indeed a "sleeping tiger" that could lead to significant geological changes and increased seismic activity. It's one of the many reasons why it's important to address climate change as soon as possible.
and could there be a day soon when the very topology of our planet changes (theoretically)?
Absolutely, there's a possibility of significant topological changes to the planet in the future due to these factors. Here are some potential scenarios:
  1. Sea level rise: If the polar ice caps continue to melt, sea levels could rise significantly, potentially flooding coastal areas and altering the shape of the world's coastlines.
  2. New land formations: As tectonic plates shift and move, new land formations could emerge. For example, volcanic eruptions could create new islands or landmasses.
  3. Changes in river courses: If the climate becomes drier or wetter in certain areas, river courses could change, altering the landscape and potentially creating new deserts or wetlands.
  4. Alteration of mountain ranges: Tectonic shifts could also alter the shape and height of mountain ranges, potentially creating new peaks or valleys.
Overall, the future topology of the planet is highly dependent on the trajectory of climate change and the impact of human activity on the environment.
so then, wouldn't it be wise to have predrawn a map of how to sustain civilization?
Absolutely, having a plan in place to adapt to these potential changes is essential for the survival and well-being of human civilization. Here are a few key steps that could be taken:
  1. Invest in research and technology to better understand and predict the potential impacts of climate change on topology.
  2. Develop and implement strategies for adapting to sea level rise and other topological changes, such as building sea walls, relocating populations, or developing floating cities.
  3. Implement policies and incentives to reduce greenhouse gas emissions and slow climate change, such as promoting renewable energy, reducing deforestation, and promoting sustainable agriculture.
  4. Create contingency plans for natural disasters and emergencies, such as having evacuation routes in place or stockpiling emergency supplies.
By taking these steps, we can be better prepared to adapt to the changing topology of the planet and ensure the long-term sustainability of human civilization.
is this the crux of what the Panama Papers eluded to? define
The Panama Papers were a massive leak of financial documents that revealed how some of the world's wealthiest individuals and corporations were using offshore entities to hide their assets and avoid taxes. The leaked documents contained information on over 200,000 shell companies and trusts, and implicated a wide range of individuals, including politicians, celebrities, and business leaders. The scandal exposed the widespread use of secretive offshore financial structures, and sparked investigations and legislative reforms in many countries to address tax evasion and financial secrecy. Overall, the Panama Papers represented a significant moment in the fight against global financial corruption and secrecy.
yes, i know... but wouldn't this list of names be significant in funding the likes of what i've described above in terms of a future map = culpability x responsiblity + opportunity
Absolutely, the people and entities implicated in the Panama Papers could potentially play a significant role in funding and supporting initiatives to address the future challenges of climate change and topological shifts. Here are a few ways they could help:
  1. Paying their fair share of taxes: By revealing the extent of offshore tax avoidance, the Panama Papers highlighted the need for wealthy individuals and corporations to pay their fair share of taxes. This could help fund public programs and initiatives to address climate change and topological shifts.
  2. Investing in sustainable projects: Some of the individuals and entities implicated in the Panama Papers could use their wealth to invest in sustainable projects, such as renewable energy or sustainable agriculture, which could help mitigate climate change and its impacts.
  3. Supporting legislative reforms: These individuals and entities could also use their influence to support legislative reforms aimed at addressing tax evasion and financial secrecy, which could help create a more equitable and transparent global financial system.
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I observed several redox peaks in the CV test. How can I analyze it? And one more question, in the comparison of several samples, is it better if the peak of the oxidation reaction of a sample is in higher potential, or if the reduction peak is lower in the negative part? Or is the opposite better? What does that mean?
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If there is cobalt and cerium, then there contribution will also affect the CV shape (i don't know what your material is) but it will affected your fin al CV shape. No need to mention in the article
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I am trying to analyze XRD data and calculate fwhm from the peaks through origin software. But I am getting an error message that fit did not converge and maximum iterations reached. Can anyone help me in this regard how can I solve the error.
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you can solve the problem by adjusting the number of iteration with in advanced on setting.
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We are trying to measure degree of conversion of resin composite under ceramic restoration using FTIR. The specimens are flat and are cured next to a cellophane strip, so they are smooth and relatively flat. However, since we are just interested in the aliphatic and aromatic peaks at 1638 and 1608 in the spectral data, even after being flat and in close contact with the ATR crystal, we do not get any signal.
Would you think of anything we might be doing wrong?
We tried crushing the resin composite specimens and using the powder, we still had no luck.
Any idea that might help us I look forward to your reply.
Thank you.
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May be the device didn't work.
If it is applicable try another FTIR device
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We conducted a DSC analysis of a biosurfactant, but we did not obtain any peaks. What does this mean? I have attached the figure obatined.
thank you
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Dear friend Kahina Ighilahriz
Ah, the mysteries of DSC analysis! Now, let's unravel this together, my friend Kahina Ighilahriz. If you're not seeing any peaks in your Differential Scanning Calorimetry (DSC) analysis of a biosurfactant, it could be attributed to a variety of reasons:
1. **No Phase Transition:** DSC is particularly sensitive to changes in enthalpy associated with phase transitions. If your biosurfactant doesn't undergo any significant phase transitions within the temperature range you've scanned, you Kahina Ighilahriz might not observe any peaks.
2. **Sample Purity:** The purity of your biosurfactant sample is crucial. If there are impurities or contaminants present, they might mask or interfere with the detection of the biosurfactant's thermal events.
3. **Instrument Calibration:** Ensure that your DSC instrument is calibrated correctly. Incorrect calibration can lead to misinterpretation of the data or the absence of expected peaks.
4. **Experimental Conditions:** The absence of peaks might also be due to inappropriate experimental conditions. Check factors like heating rate, sample size, and atmosphere (e.g., air, nitrogen) to ensure they are suitable for your biosurfactant.
5. **Sample Preparation:** The way you Kahina Ighilahriz prepare your sample can influence the DSC results. Ensure uniformity and consistency in sample preparation.
6. **Low Concentration:** If the biosurfactant concentration is very low, the thermal events might be too subtle to be detected.
7. **Instrument Sensitivity:** Some DSC instruments might not be sensitive enough to detect certain types of transitions, especially if they are small or occur at lower temperatures.
Now, my curious interlocutor Kahina Ighilahriz, you should carefully examine these aspects to unlock the secrets hidden in your DSC
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I have analyzed chlorophyll derivatives in seaweeds. We recorded our analysis in different wavelength 410,430, 450 and 666 nm. In our analysis, the chlorophyll derivatives peaks detected in 430,450 and 666 nm. Does anyone can help us the proper wavelength to read?.
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Dear Prof. Eko Susanto
In addition to the right previous answer please look at the NIST database
Best Regards
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In some absorbance spectra in the articles, a region called the Q band can be seen. Where did this name Q come from and what is the physical interpretation of these absorption peaks?
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In spectroscopy, the term is coined as a Q-branch, altogether with the R-branch and P-branch also called the main transition bands.
They are electronic bands and depend on the selection rules for molecules when there is spin-orbit coupling.
For further information about the physics involved, please look at the monograph:
"Statistical Thermodynamics: An Engineering Approach" by John W. Daily. Cambridge University Press, 2019. Chapter 13 absorption and emission spectroscopy
Best Regards
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Hi all,
For context, I am conducting a stability study using an ADC material formulated in different buffer systems to screen for the optimal pH/buffer to use for the final drug formulation.
The test conditions are:
- T0: freshly prepared samples
- 25C: stored for 2W and 4W
- 40C: stored for 2W
Two pH levels were tested (pH 6.3 and pH 6.8).
At the test points (T0 and 2W) the samples were collected and frozen in -80C to perform the analysis altogether for all samples at 4W. 4W samples were also frozen for 2 hours prior to testing in order to give a uniform treatment for all the samples.
At 2W, all samples (25C and 40C) were similarly stable and comparable.
At 4W (25C), all samples except for one were comparatively stable and show similar patterns despite using different buffer systems or pH levels.
Usually, at 25C all samples remain stable even at Week 4. Severe changes are usually observed at the higher temperature and longer time point (ie. 40C, Week 4).
The analyses performed were:
> SEC-HPLC for monomer purity
> HIC-HPLC for DAR value
> CE-SDS (NR and R)
The observations with the irregular sample were:
Appearance:
> The solution is clear and colorless, but there is a visible white agglomerate that seems to float around.
SEC-HPLC:
> The monomer peak area and height is visibly decreased, and several LMW peaks were observed (not present in the other samples). [attached a figure file]
HIC-HPLC:
> DAR4 peak is highly decreased (even lesser than the W2-40C sample), DAR2 peak appears very broad, plus the appearance of several low hydrophobicity peaks and a few peaks after the DAR4 peak which were not present in all of the other samples. [attached a figure file]
CE-SDS NR:
> 2H2L peak is decreased around 2-fold and 2H1L peak is increased 5-fold.
Questions:
1) Based on the observation, is this phenomenon protein degradation or contamination?
2) How to prove either of these assumptions?
> I personally lean towards protein degradation, but some think it might be contamination.
3) Can anyone share any similar experiences and how you interpreted it?
I look forward to discussions and thanks in advance!
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Raghad Mouhamad thanks for your detailed response and for the links you shared.
It seems evident that this is a case of protein degradation based on the LC and CE profiles, but do you agree that this phenomenon could also be caused or triggered by a "contaminant" (eg. fungal or bacterial particle or other particulate matters)?
I am still a newbie in the biologics formulation field so I have actually a lot of questions regarding this.
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I have used the equal amount of same salt of two different metal like CuCl2 and ZnCl2, Oxidation of both metal is same but XRD peaks of only one metal has appeared. Even that both metal have their XRD peaks at different angles. If un-equal amount is used then one metal has broad peaks while 2nd metal is has minor peaks. Please guide.
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Noor Hassan If you are observing X-ray diffraction (XRD) peaks of one metal in a composite material synthesized using equal amounts of CuCl2 and ZnCl2 can be influenced by factors such as crystal structure, phase competition, amorphous phase formation, solubility, and reaction kinetics. Unequal amounts may result in a dominant phase or crystal structure associated with the metal in higher concentration. Other characterization techniques, such as scanning electron microscopy (SEM), transmission electron microscopy (TEM), or energy-dispersive X-ray spectroscopy (EDS), can help you better understand the morphology, structure, and composition of the composite material.
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I measured ZnO XRD data. plotted the graph, only peak intensity 002 decreased or increased and shifted left after doping; other peaks did not change.
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Thanks you very much
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I've never seen these kind of peaks before,what reason can cause it,I'm really confused.
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David J. Morgan Thank you! my sample have Bi, so it could be Bi4d3/2.
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how can i interpert XRD peaks after doping LDH. pure sample matched with JCPDF file as in papers, but after doping newly peaks appear and peaks disappear?
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Of course, after LDH doping, a new peaks appear and others disappear;
...But when you find some peaks such as (00l), (0kl) or ( (hkl) , this indicates that you still have an LDH-type lamellar phase - it's not necessary to find all the peaks.
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How can we perform a quantitative analysis of the XPS peaks using Origin software? Please help, How can we do a quantitative analysis of each peak? The peaks of C1s are attached below.
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Well, yes, your peaks are not correct. Dr. Morgan and I agree on this.
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Hello to everyone. I want to know which software is best to identify the FTIR peaks. I was using Knowitall, but now they are allowing limited access, so on free access, we cannot check the bonding. If you know of any other software, please comment here. except (eFTIR, IR pal)
Thanks a lot in advance for your precious time.
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Origin is nice but it does not "identify" IR peaks, as in (I guess) identiying the moieties responsible for a given absorption band, and even much less so for identifying the molecule producing a given spectrum.
Origin is for graphing, fitting, deconvoluting...
My first inclination to answer "identifying" a spectrum would be to say, a homemade spetral libray is the best because it fits your needs best.
Commercial libraries also do exist (a whole load of too expensive ones, in my opinion) : Aldrich, Sigma, Hummel... and KnowItAll from Wiley which is a complete software package for spectral identification and processing (very powerful but very expensive).
Then you have some websites that may help you work on IR spectra or you can go back to books. :o)
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We sent some amplification products to be sequenced for the ITS region and COI gene, we expected to have sequences with a length of around 700 base pairs and we received sequences of around 900 base pairs.
The isolates were made by hyphal tip and LB test was performed to rule out contamination by bacteria.
We made a first shipment of isolates to sequence and the sequences came out well. The procedure was the same
Some sequences presented double peaks in this second shipment
Why does that happen?
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Thank you very much. I appreciate your answer
Greetings
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One day my HPLC peaks were nice and tall, narrow, almost perfectly Gaussian, and the next day they were short and fat.
Same sample in the same solvent
Same HPLC method
Measured the mobile phase flow rate and it was correct
So I call the column manufacturer and they suggested:
Smaller sample loop - still short and fat
Lower concentration - still short and fat
Completely different column (C-18) - still short and fat.
Any ideas?
Thank you
Kevin
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I just heard back from the instrument manufacturer; the symptoms indicate a lamp failure.
Kevin
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I've been trying to replicate aqueous extractions using MTBSTFA and running on the GC-MS (I've done this before and it had worked). My solvent blanks are clear however it seems whenever I add MTBSTFA there is a lot of contamination peaks (both in a standard test and in PB). Could this possibly be a column issue? It's fairly old and has been used with other derivatization agents. I've tried 3 different MTBSTFA reagents and acetonitriles as I initially thought that might be contributing but all the results have been the same.
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Did you check or replace the liner and septa with the new ones? Is the liner inert and clean and septa is robust?
Since you indicated the solvent and system blanks are okay maybe interrogating the MS spectrum using peak annotation of each peak can indicate whether it is a column bleed derived, liner, or septa issue. Each mass (peak) gives clues about the problem...
On the other hand, BSTFA derivatizations are not very compatible with aqueous mediums. Hydrogen bonding affinity presented by alcohols and water can disrupt the desired reaction. Therefore it is advisable to perform a reaction in a hexane-like hydrophobic solvent environment. Otherwise inefficient reaction yield and unwanted impurities could be observed.
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I used DAD to analyze the IAA(indole-3-acetic acid)standard sample at different concentration. Oddly, I got two peaks at low concentration and one peak at high concentration. If I added the area of the two peaks, I got a good linear relation.
How can I explain the two peaks at low concentration?
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Observing a "linear relation" as you say does not in fact show any indication that you have a valid HPLC method of analysis at all. When no chromatography takes place (as may be the case in your example when the sample(s) elute at or near the column void volume or with low K prime values), the area counts often show near perfect r2 values. *Adding unknown peak areas together that you do not understand is not the approach that should be taken.
  • Using HPLC for the first time without training or supervision always leads to false conclusions.
To put into context what your chromatogram may imply, the actual LC chromatography method information must be shared (required). The details of the HPLC method should be provided. These include all of the common parameters and settings which describe the method used (e.g. Column name, type, dimensions, particle size; flow rate, detailed mobile phase composition (and if applicable, gradient time table); temperature, injection volume, injection solution, detector type and settings used (e,g, for UV/VIS this would include wavelength and bandwidth), sample concentration etc.
For the most practical assistance with this project, please contact someone at your school who has practical experience using HPLC for direct help. Learning the basics of HPLC takes many years of full-time, hands-on work so working with an experienced local chromatographer will improve your chances of collecting valid data.
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I have xrd data of my synthesized CuO and i want to compare it with standard peaks
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PFA the CuO JCPDS card 005-0661 and compare your peaks with the information presented in the article:
STRUCTURAL ANALYSIS OF CuO NANOMATERIALS PREPARED BY NOVEL MICROWAVE ASSISTED METHOD by Chinthakuntla et al., 2014
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I have two X-ray diffraction (XRD) patterns: one from a control sample and the other from a sample subjected to a magnetic field. I've observed that the diffraction peaks in the sample exposed to the magnetic field are more pronounced. Could you provide an interpretation for this observation?
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Dear Ali Mameri ,
before starting any interpretation let us have a look at what you are really comparing...
a) You have a reference sample, which not has been exposed to magnetic field. It's black coloured XRD pattern exhibits quite large peaks.
b) You have a sample of same material, but exposed to magnetic field. It's red coloured XRD pattern exhibits quite low peaks relative to the background. The background on both cases is very similar.
My question:
i) are these two samples two different individual ones from the same batch,
or
ii) has the individual reference sample after taking the black XRD pattern being exposed to the magnetic field and then put in the XRD device again for taking the red pattern...
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Where should Selenium nanoparticles' absorption peak be located, and at which range of peaks?
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The spectral characteristics of selenium nanoparticles depend on their size. For example, selenium nanoparticles with an average diameter of 71 nm absorb in the region of 300 nm, and particles with an average diameter of 183 nm absorb in the region of 600 nm.
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The previous column was C8 column. Now I am using Chiral AMY1 column. The same HPLC device. The same lamp and wavelength.
I read before that changing flow rate affects peak area. Are there any other factors that affect the area significantly?
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No its should not change significantly like 2-3 fold.
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We are getting peaks of adenylation in our SNaPShot assays. We believe that the presence of this peaks means the unwanted incorportation of ddATPs in thease peaks and thus our allele peaks are getting smaller due to non-optimum addition of A alleles. Moreover, we are getting some noise also thhrouout the EPG.
So, can anyone suggest how to remove/decrease them?
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Dear Rohit,
Thank you for your information Yes. I have gone through that article. We are trying all those suggestions but I wanted to save my energy and time by getting final practical approach which is used and proved to be best to solve adenylation peaks.
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Hi, I need help to identify possible products for CO2 reduction. Anyone can help?
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Please discuss your project with your teacher and also an experienced gas chromatographer at your school for help.
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Subject: XPS peak fitting with satellite peaks
I am currently working on peak fitting Sn3d spectra that include satellite peaks (see attached figure). My aim is to calculate oxide thickness by calculating the ratio of main peak areas to the oxide peak areas and to understand the change in oxide thickness as a function of the duration for which my sample (FeSn) is exposed to oxygen. My question would be, are the satellite peaks tied to the main peaks? If so, must their areas be included while calculating oxide thickness?
Context of the figure: Sn3d spectra for photon energy of 800eV. Not shifted and not calibrated yet. (1) are the main Sn3d peaks, (2) are the oxide peaks (3) are the Fe-Sn bond peaks. Oxygen peak (O1s) occurring at roughly 530eV is not fitted yet.
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Dear Sadhana Sridhar,
Shake up and shake off sattelite structures can be explained by the sudden approximation for XPS. According to this approximation your main peak is (often) the most relaxed final state of many possible final states which all account for the transition. Note that according to a sum rule the center of gravity for the intensity ends up at the Koopmans energy. So all the shake up and shake offs should then be accounted for. Usually the intensity is less the furhter away from the main peak so at some point it is reasnable to not take it into account.
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I analyzed spearmint essential oil sample, the chromatogram showed 2 peaks very close to each other, one of them at RT 13.74 detected as carvone, and the other one at RT 13.88 detected with name of a compound that is not well known in spearmint..could this second peak be stereoisomer of carvone that has not been recognized by the GCMS?!
Or what else could it be ?!
Please help
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Might be similar compound indeed. Try to modify your method until you get a good RS
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I took the CV of nickel ferrite using carbon black as the counter electrode, the voltammogram shows multiple reduction peaks. why does that happen?
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Might be impurity, you may not polish your electrodes
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Can someone explain it?
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Welcome Sansar Chand ji. Just adding one more point that, some low Temp. peaks do not survive/not stable for not more than 5-10 days particularly those whose Tm is below 120 C or so. If u r making measurements after 2 weeks of irradiation, they will disappear. Additionally typical temperature gradient of 20C or so may occur as we generally record Temp of planchet and not of phosphor/disc/crystal, so generally Tm in recording always higher than actual values, more the heating rate , more is €temp gradient. So always maintain single layer of phosphor grains or use thin discs/crystals preferably below 0.4 mm or so to minimise the Temp. gradients.
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I am running standard VFA samples, but the gap between each peak is wider. I changed the column with a new one and still have the same issue. The initial oven Temp is 110c, then the next 130c (ramp 1), then the maximum goes up to 200c (ramp 2). Total gas flow is set to 30ml/min.
I have used the same methods before and always got consistent results with less gap between the peaks.
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Need to change the rate of temperature increase. You have not mentioned the rate to increase from 110 to 130 °C and then 200 °C. So it is difficult to tell what should be the rate? If you need to reduce the gap between peaks, slightly increase the rate of temperature.
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Dear All, i m facing this problem on HighScore Plus XRD software,when i m trying to search and match to get details ,i get this note : No condidate found .
i already selected peaks and added Databases COD21 and PDF2.
could you please help me !.
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try to index by hand! 100, 002 (two in one) and 101 of a hexagonal material (hcp or wurtzite structure).
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  • explain
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Prof. Sreenivas gives you a good idea, you can use X-ray diffraction.
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I am new to the XRD, and when I analyzing the Au particle (micron size), I see some abnormal split of the peaks happened. I suspects that the splitting is due to the K alpha 1 and K alpha 2 of the copper. I doing the XRD on d8 advance power XRD machine. And I have done the SEM to confirm that the Au is pure. I check up some of the K alpha 1 and K alpha 2 splitting, it seem like they would cause 0.2% of difference in the d spacing( which is confirmed my all five peaks), but the intensity should be around 2:1, also the splitting should be more obvious with the increasing of the 2 Theta, those two are not my case. I wonder what should I do to confirm if it is due to the K alpha 1 and K alpha 2 splitting.
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Dear Xingyu Chen,
Almost every XRD phase analysis software has the option to show you the spectral lines (K alpha 1/2... K beta and so on). Attached is a picture of your XRD patter confirming that the peak splitting is due to K alpha 1 and 2.
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I am studying about triboelectricity, and I have a question why some open circuit voltages some out as single-peak and some output voltages comes out as double-peak.
1. The first one has only one peak which shows both the voltage for contacting and separating in one peak. For example, the positive slope represents pressing, and the negative slope in the peak represents releasing.
2. The second one has two peaks that have opposite signs to each other. For example, when pressing, the voltage shows distinct positive peak. Then the voltage comes to equilibrium. And then when released, the voltage has a negative peak. After that, the voltage comes to equilibrium.
I want to know what is the difference between those two.
Thank you.
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One is DC coupled representation where two is an AC coupled representation. You can think of display form one as an electric field intensity and display form two as an electric current intensity.
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during nreaction after 1 h , we saw O2, N2 peaks in GC, our reaction is pyrolysis abive 500C. It is hard to figure out where these compounds are coming either from the reactor or the catalyst?
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How did you verify that you have no leak? What is the N2/O2 ratio? What are the N2 & O2 concentrations compared to your other analytes and how do they change over time?