Science topic

Inorganic Synthesis - Science topic

Explore the latest questions and answers in Inorganic Synthesis, and find Inorganic Synthesis experts.
Questions related to Inorganic Synthesis
  • asked a question related to Inorganic Synthesis
Question
9 answers
We need a complex of the form M+PF6-. We tried to synthesize along with the reaction using NH4PF6.  But its not forming. Is there any way to form the complexes of this type. Kindly refer some papers..
Thanks in advance
Relevant answer
Answer
Dear Derek Would you recommend silver for exchanging K+ for Li+ for getting LiPF6? Thanks in avance
  • asked a question related to Inorganic Synthesis
Question
5 answers
I wish to do visible light experiments in the lab. Please suggest what type of setup (bulbs/lamps) I need to purchase? Please suggest to me, the make and the supplier of these items.
Relevant answer
Answer
use lamp
  • asked a question related to Inorganic Synthesis
Question
4 answers
Dear colleagues
pH setting such as for testing the stability of photocatalyst (or other materials) is one of the important thing. Generally, this condition can be adjusted by pouring or dropping some acid or base compound droplets like HNO3 (nitrate acid), HCl (chloride acid), NaOH (sodium hydoxide) and so on. But, I think there're some main considerations to choose one of them. Maybe, there some of you can share tips to select a proper acid and base compounds in controling pH situation especially in inorganic synthesis material, pH stability, or dye photodegradation?
Thank you very much.
Relevant answer
Answer
Hi, Febiyanto,
May be, you can first do a bibliography on your synthetic materials to assess their stability with respect to pH, which I agree with you is an important parameter during the organic pollutants degradation such as dyes.
Good luck
Safia
  • asked a question related to Inorganic Synthesis
Question
5 answers
Kindly I am asking for the possibilities of formation of transition metal complexes of Pt(II) with octahedral geometry.
If it is possible, could you help me by referring to published papers that included this type of complexes?
Thank you very much in advance.
Relevant answer
Answer
Hello,
In general, no. Pt(II) likes to be square planar. There are some examples of 5-coordinate Pt(II). Also, you can have Pt(II) with hydrogen bonding to the open sites above and below the square plane, but that's not technically ligand coordination.
Sincerely,
Kyle
  • asked a question related to Inorganic Synthesis
Question
5 answers
I have gone through many publications, books for eg: Powder diffraction files, Inorganic phases and Marine Manganese deposits by Glasby etc. and also online in webmineral data but could not identify few minerals from its d-spacing value and 2theta angle. So maybe someone can help me out with the attached mineral data in excel sheet:
 
Relevant answer
Answer
Can anyone help me identify the minerals of the attached files, i was only able to identify quartz using match but i cannot identify anything else, please advise/help
  • asked a question related to Inorganic Synthesis
Question
2 answers
I'm thinking about Na2S, but I was wondering if using any organic reagent like thiourea (it should thermally decompose at low temperatures) would be suitable too? Thanks
Relevant answer
Answer
To obtain thin CdS layers of 50-70 nm, I used thiourea. The SILAR reaction was carried out at room temperature.
  • asked a question related to Inorganic Synthesis
Question
14 answers
I am working on metal organic polyhedra topic to synthesize new metal-organic cages or other based frameworks. I want to conduct postsynthetic modification for one cage, but the solubility is very poor in most solvents, only methanol can dissolve but it needs large volume.
My question for who in the field of MOFs, COFs, MOPs, and other related chemistries, how can I deal with the problem of insolubility of synthesized materials to conduct postsynthetic reactions? what are the proposed strategies and methods to attain the target modified compound?
Relevant answer
Answer
Reactions can be of different types: addition, substitution (nucleophilic or electrophilic), acid-base reactions [adduct formation, coordination complexes], metathesis, transmetallation etc., One should examine the nature of the compound and what interactions with solvent will enable the compound (solute) to dissolve in it.
Some time reactions can be carried out in solid state by using finely divided particles (grind well in a mixer or using pestle-mortar to increase the surface area) using ball milling (popularly known as mechanochemical method).
Also one can use a solvent in which the reactants are insoluble but still reaction can happen.
If needed use more solvent and generate suspension and reaction can occur.
If it is sparingly soluble in methanol, still reaction can be carried out.
If it is ionic complex, try to substitute the anionic species with a better anion and that should help. If the complex is an anionic species, try to encapsulate the cation using polyethers, cryptands etc. to make it soluble in polar organic solvents.
  • asked a question related to Inorganic Synthesis
Question
5 answers
Sometimes geopolymers are said to have N-A-S-H (sodium aluminium silicate hydrate in the cement chemist notation) gel as the binding phase. I was wondering what is the difference of N-A-S-H and zeolites if any? Zeolites are also frequently present geopolymers and they are also aluminium silicates with hydrated sodiums.
Relevant answer
Answer
I put more words, in addition to Carlos response. Zeolites are highly crystalline (mostly), whereas other aluminosilicate counterparts are amorphous in nature. Zeolites possess high Si to Al ratio compared to geopolymers (lower than 2-3). Zeolites are micro and mesoporous with higher SSA whereas pure geopolymers are low in SSA (mesoporous). Zeolites are more organised framework and cage and pore confinement. I share more ideas how to improve key properties of geopolymers which can be utilized similar way like zeolites.
  • asked a question related to Inorganic Synthesis
Question
3 answers
Hello,
I'm trying to use 2,6-Naphthalenedisulfonic acid disodium salt for synthesis of some inorganic clusters. But having difficulties to make it soluble in water. The manufacturer website said it's miscible in water and should be a white powder. But I purchased it from different vendor and they are kinds of dirty whitish/brown powder and forms brown color solution with dirty coagulant like precipitate (at 0.1M).
Please let me know if someone is facing the same issue and know the strategy to solve the problem.
Thanks,
Shohel
Relevant answer
Answer
Hi,
As you mentioned that you purchased from a different vendor and it doesn't have same physical appearance that simply means that it is adulterated with some impurity which might hinders its solubility in water.
The only way is that you dissolve your impure compound in water and then filter the resulting mixture. I believe that the salt will solubilize in water whereas the impurities will filter out. Later you can check the concentration of salt in filtrate.
Good Luck
  • asked a question related to Inorganic Synthesis
Question
11 answers
Ruthenium(III) Chloride, Anhydrous with high assay is not so expensive. Hydrate is hard to measure the exact Ru content. However, hydrate is used for the synthesis of Ru nanoparticles. Wikipedia also says it (https://en.wikipedia.org/wiki/Ruthenium(III)_chloride). What is the advantage of using hydrate?
Relevant answer
Answer
The anhydrous RuCl3 is chemically inert and has very low solubility to most of the solvents.
  • asked a question related to Inorganic Synthesis
Question
4 answers
I want to get (C6H5)2PNa but unfortunately in the lab only have (C6H5)2PCl as a reagent. in adition we have Na and the common solvents.
my question is really about the feasible of the reaction
(C6H5)2PCl + 2Na ----> (C6H5)2PNa + NaCl
what are the optimal conditions for the reaction above?
Relevant answer
Answer
Synthesis of (C6H5)2PNa:
For the preparation of the sodium diphenylphosphine they were placed in a two-mouth balloon, supplied with a refrigerant and an ampoule of addition, 200 mmol of Na metal in small pieces in 75 ml of dry dioxane under Argon or Nitrogen!! Then they were added slowly and under constant agitation 40 mmol of diphenylphosphine chloride, (C6H5)2PCl. Once the addition was complete, the mixture was placed under reflux by 5 hours in which a yellow solid insoluble in dioxane was produced. The mixture was allowed to cool and the product was extracted by adding 50 ml of dry tetrahydrofuran, THF, in which it is soluble. Excess sodium will be separated by filtration on a fried plate and then evaporated the solvent obtaining an orange-yellow solid. Sodium diphenylpshopide gets easliy oxidized by air.
  • asked a question related to Inorganic Synthesis
Question
6 answers
I would like to know, while synthesising lithium containing oxides (solid electrolyte), was there a loss of lithium content (very much less in content, than anticipated, in the obtained product)?
In order to overcome this, what all techniques were tried.
Relevant answer
Answer
Dear Athul,
1) how did you measure the (low[1]) conductivity ?
2) What are your (Li?) electrodes[2] in measuring the (low[1]) Li-ion conductivity ?
A simple proposal method to estimate the Li-conductivity is to implement EIS[4] using a thin[5] possible (the thinner the better) sample (sample's sandwich) of your solid electrolyte. So, prepare a thin sandwich among two (same: Li, or even Cu, Al, inox[6], etc.) metal electrodes and measure EIS[7] spectra. Then, make a good estimation of the (Li-ion, only) conductivity, implementing a model[4,7].
1. Your declaration (-believe) is not always decisive : We were successful in synthesizing[2,3] the compound, but the lithium content was pretty low. Which in-turn, we believe(???), might have reduced our compound's ionic conductivity.
2. Mastering the interface for advanced all-solid-state lithium rechargeable batteries http://www.pnas.org/content/pnas/113/47/13313.full.pdf
3. Solid-state electrolyte with lithium-ion conductivities comparable to liquid electrolytes https://phys.org/news/2017-09-solid-state-electrolyte-lithium-ion-liquid-electrolytes.html
5. Negligible “Negative Space-Charge Layer Effects” at Oxide-Electrolyte/Electrode Interfaces of Thin-Film Batteries https://pubs.acs.org/doi/10.1021/nl5035896
6. Effect of succinonitrile on electrical, ... LiI–I 2 redox-couple solid polymer electrolyte
  • asked a question related to Inorganic Synthesis
Question
1 answer
I know these are often arc-welded under Ar. My question is more specific. Are the ampules crimped before sealing? Does the crimping compromise the strength of the tube? What thickness of Ta or Nb is used? Is the ampule fashioned from Ta or Nb tubing? What companies sell affordable Ta or Nb for this purpose? After the reaction, how is the ampule opened? Thank you,
Dan
Relevant answer
Answer
If a certain medium (inert gas) is required for the reaction, the tube with the sample must be connected by appropriate rubber vacuum tube to the pumping and the gas filling system before welding. Use the smallest flows, otherwise all the contents will be in the pump! After pumping and filling with gas, the tube must be clamped tightly (at least 135 deg., this must be done so that the edge is available for cutting and welding), cut off and the edge will rolled up. After the experiment, cuts the welded edge (without water cooling!) by compact disk cutter.
Now electron beam welding (under microscope) is often used.
Recommendation: The inner wall of the tube, especially in the area of future welding, must be thoroughly cleaned both before and after the sample loading. Then the tube (until the end of welding) should always be in an upright position. You can use a suitable stand for this. Pipes are taken from a neighbor laboratory (the easiest way), or it is necessary to search on the Internet. Pay attention to high-tech enterprises related to space, etc. Do not trust completely the purchase manager of your institute; in this case, you have a serious chance to get titanium or even stainless steel tubes. It makes sense to talk with the supplier's manager about the refuse or defect (short, damaged or crumpled tubes), as it should be cheaper, and sometimes it is available, even if they do not sell quality tubes as product. The thickness should be 0.2 - 0.6 mm. It is difficult to work with thicker material. I worked a bit with niobium and tantalum (only wires and foils), but pure molybdenum and tungsten (well known to me) are very fragile, only one fold allowed.
The result will depend on the thoroughness and planning of all procedures.
  • asked a question related to Inorganic Synthesis
Question
3 answers
In several solid-state synthesis and sol-gel synthesis for similar compounds, sometimes NH4H2PO4 is used and sometimes (NH4)2HPO4 is used instead.
I would like to find out if it is one chosen randomly and could be substituted by the other one or there is an explanation why one is chosen.
I already know their differences in acidity and that P-O bonds where the O is protonated are longer and rarely forms coordinated bonds, but I would appreaciate a further explanation for the aforementioned issue.
Relevant answer
Answer
(NH4)2HPO4 + HOH = NH4OH + NH4H2PO4 pH 0,1 M = 8 NH4H2PO4 + HOH = NH4OH + H3PO4 pH 0,1 M = 4,4 3NH4+ + 3HOH = NH4OH + 3H+
Which salt to choose for synthesis depends on the pH of the synthesis. As you can see (NH4) 2HPO4 forms a neutral medium as a result of hydrolysis, and NH4H2PO4 is acidic.
  • asked a question related to Inorganic Synthesis
Question
5 answers
I need to determine the copper (II) content in a powder with a relatively simple method. I plan to: (1) extract the copper (II) from the powder by digestion with nitric acid; and (2) titrate the copper (II) solution with disodium EDTA after adjusting the pH approx. 4 with an acetic acid/sodium acetate buffer. I plan to use alizarin as an indicator as it changes colour at pH 4.3.
I am also considering using an iodometric titration, which involves reacting the copper (II) with excess iodide and titrating the iodine produced with sodium thiosulfate.
Can anyone comment on these plans in terms of: advantages of disadvantages; factors I need to be aware of; or changes I need to make?
Relevant answer
Answer
Iodometric titration of copper is a simple and low cost method to determine copper content. If you google the topic you will find many easy procedures employing chemicals you probably have in your laboratory.
  • asked a question related to Inorganic Synthesis
Question
3 answers
The O-debenzylation by using TiCl4 is mentionned in several papers but any of them describes the mechanism...
Relevant answer
Answer
thank you so much
  • asked a question related to Inorganic Synthesis
Question
4 answers
i used ascorbic acid as stabilizing agent and sugar as reducing agent i try variable ratios of metal ligand and ascorbic acid and vaying ph for stability but fail to stabilize after 4 hour of synthesis the of nanoparticles which are orange beomes change to orangish brown and peak becomes diminish i tried ph up to 13.8
first I  mix metal ligand and ascobic acid stir and heat solution for 15 minutes cool solution then maintain ph  up to 13.8 (the nps synthesize  ph  between 11.5-13.8) during maintaing Ph the color of the solution changes to dark yellow stir the solution up to 10 minutes the colour changes to orange the wavelength between 500-510nm. file is attach i dont to change my ligand plz give valueable suggestion
Relevant answer
Answer
Try the reaction in water free environment. Use organic solvents.
  • asked a question related to Inorganic Synthesis
Question
5 answers
See above
Relevant answer
Answer
Tabulated values for the density of ZnCl2 aqueous solutions, at temperatures ranging from 0 ºC to 100 ºC, can be retrieved from (e.g.): R.H. Perry, D.W. Green, J.O. Maloney (Eds.), "Perry's Chemical Engineers’ Handbook", 7th ed., McGraw-Hill, 1997, cf. Table 2-103. 
  • asked a question related to Inorganic Synthesis
Question
2 answers
Hello all,
I would like to ask you if anybody has any input on the reactivity of gaseous nitrosyl chloride towards acetonitrile.
I wanted to perform a methathesis reaction between NOCl and a weakly coordinating salt of sodium in acetonitrile and would like to know whether my approach is save to handle or just irresponsibly hazardous.
The idea was to bubble NOCl through a solution of the sodium salt in acetonitrile, hoping that sodium chloride would precipitate out and leave my nitrosonium ion with the weakly coordinating ion in solution.
Thanks in advance for any information provided!
Relevant answer
Answer
CH3CN is always contaminated with water. It's very difficult to get dry acetonitrile. NOCl is sensitive to water.  NO+ is a very strong oxidant with Eo about 1.8 V (NHE).  All chemical experiments are potentially dangerous. Material safety data sheet:
 My major concern in your question is: "a weakly coordinating salt of sodium in acetonitrile." I really do not know which sodium salt is soluble in CH3CN.
  • asked a question related to Inorganic Synthesis
Question
3 answers
Inorganic synthesis
Relevant answer
Answer
I agree with the opinion of the upper storey ,you can verify it .
  • asked a question related to Inorganic Synthesis
Question
4 answers
Can metal acetate work as an oxidizing agent in DMF?
Relevant answer
Answer
thank you all for your suggestions. Actually i have a ligand that doesn't have any metal when i am refluxing it in DMSO with Nickel acetate then nickel is cordinating to the ligand and ligand itself oxidizing
  • asked a question related to Inorganic Synthesis
Question
3 answers
I am synthesizing zinc aluminate these days with zinc nitrate , aluminum nitrate and ammonium hydroxide by co-precipitation method. However, because zinc ions can form complex ion with NH4+, the powder I synthesized always has excess aluminium oxide, which can be seen from XRF, but i can't find peaks of aluminium oxide in XRD diagrams.So how can I synthesize stoichiometric zinc aluminate?
Relevant answer
Answer
See the article enclosed, for an alternative synthesis method.
Best wishes,
Carlos
  • asked a question related to Inorganic Synthesis
Question
1 answer
Is there a simple procedure to make Gallium sulfate from Gallium metal? I used Gallium metal and sulfuric acid ~ 2M; but the reaction is extremely slow.
Relevant answer
Answer
try using cocn H2SO4 98% (cheap and comercially availible just add through a droppiong funnel slowly!! ) this should speed this up significantly or heat it until reflux
check this refrence out to form it from the chloride  DOI: 10.1021/ja01286a011
The Precipitation of Basic Gallium Sulfate by Means of Urea. I. A Study of the Precipitate Produced Hobart H. Willard, H. C. Fogg J. Am. Chem. Soc., 1937, 59 (7), pp 1197–1199
or alternatevely disolve gallium chloride in toluene or hexane and add conc H2SO4 ( this liberates HCL gas)  and should form the sulfate
the sulfate is also comercially available from sigma aldrich
hope these help
J
  • asked a question related to Inorganic Synthesis
Question
3 answers
The reaction is in DMF and the resulting products are easily dissolved in water.
Relevant answer
Answer
Try a different solvent (DCE or EtOAc) and/or filter through a plug of silica or alumina. 
  • asked a question related to Inorganic Synthesis
Question
13 answers
I am attempting to exchange nanoparticle's surface ligand (oleic acid) with another ligand (i.e., citric acid). However, the product yield is too small to get it in powder form and not enough to be measured by FTIR. In that case which tool(s) would be suitable to get the information of exchanged ligand.
N.B.: product is stored as colloidal form.
Relevant answer
Answer
ATR-FTIR.The method is very simple and requires a small drop of your sample.
  • asked a question related to Inorganic Synthesis
Question
4 answers
Can any one please suggest me reducing agent names for reduction of chlorides?
for example: Cucl2+reducing agent >>copper or copper oxides.
please give me the chemical equations and mechanism.
Relevant answer
Answer
Ah, you want to reduce a metal cation? You should say this, if you know what I mean.
  • asked a question related to Inorganic Synthesis
Question
2 answers
The MLCT bands of the fac-Re(CO)3-core Complexes are having less wavelength values than that of the fac-Mn(CO)3-core complexes. What might be reason and what will be the explanation for this ?. Please help me in this regards. If possible please suggest the reference for this content.
Thanking you. 
Relevant answer
Answer
Lots of literature out there on this. Check out people like Kaim, Ishitani, and Hartl for papers on UV-Vis spectra of Mn and Re fac-tricarbonyls. 
  • asked a question related to Inorganic Synthesis
Question
7 answers
We are trying to substitute chloride ligand from a Ruthenium metal complex. We have tried a few methods, refluxing with MeCN/H2O or MeOH/H2O with the aim of substituting chloride, but failed every time. I would really appreciate if anyone can suggest ways in which it can be achieved. Parallely, I, myself, am looking in literature for a convenient procedure.
Thank you in advance.
Relevant answer
Answer
A classic method is the reaction with Ag+ ion. A good choice colud be AgBF4 or AgOTf.The only possible inconvenience comes from the oxidating potential of Ag+, wich can lead to oxidation of your substrate or ligands. The alternative is in using Tl+ ion.
Anyway, in the end you have to filter out AgCl or TlCl.
A more subtle approach is in using NaBPh4 in excess, if you are operating in organic solvents or mixtures (ie.g.CH2Cl2/EtOH mixtures): BPh4- stimutate the precipitation of the cationic metal complex and the formation of close ionic couples Na+Cl- together drives the elimination/substitution of Cl- bonded to the metal with another ligand, anionic or neutral.
  • asked a question related to Inorganic Synthesis
Question
3 answers
Is there a paper or can someone helpme to explain the mechanism of reaction between ethanolamine and cyclopropanecarbonitrile catalyzed with cadmium acetate dihydrate for the formation of 2-cyclopropyl-2-oxazoline, especially how is it that cadmium acetate acts.
Relevant answer
Answer
Transition metal acetates such as zinc or cadmium acetate act as a moderate Lewis acid to activate the nitrile (N in the nitrile is a Lewis base). The carbon in the nitrile becomes then more electrophilic and can be attacked by the ethanolamine. After a series of intramolecular acid-base reactions you end up with the oxazoline releasing ammonia. This is what we call the Witte and Seeliger method to prepare 2-substituted oxazolines (Liebigs Ann. Chem. 1974, 996 - 1009). Suerte!
  • asked a question related to Inorganic Synthesis
Question
3 answers
I want to make trimetallic nanoparticles of Mn-Ni-Si using chemical reduction method. I am using precursors as chlorides, for Mn and Ni it is easy to hydrate the chlorides but for SiCl4, if it is hydrated, it immediately forms SiO2 lumps in the solution. Can you suggest an alternative method for this and also the reducing agent which could be used for chemical synthesis of MnNiSi nanoparticles.
Relevant answer
Answer
Can you not use an anhydrous non aqueous solvent like DMF or THF? Admittedly, this may require alternative reducing agents -eg to generate a THF-BH3 complex from the NaBH4. But as you have discovered, you cannot use SiCl4 with any aqueous solution. One other question: do the anhydrous manganese and nickel chlorides dissolve in SiCl4?
  • asked a question related to Inorganic Synthesis
Question
4 answers
I have tried synthesizing azitidinone from imino pyridines by treating with chloroacetyl chloride in the presence of triethylamine, using 1,4-dioxan  as a solvent. but no change in the starting material is observed. Please suggest me suitable method for the synthesis of same.
Relevant answer
Answer
Best method to synthesize azitidinones(B-lactum) from imines is the cycloaddition reaction of imines with ketene intermediate .Imine rects with chloroacetyl chloride in presence of triethyl amine gives Beta lactum.
  • asked a question related to Inorganic Synthesis
Question
1 answer
which is the best combination of redox electrolyte for DSSCs?
ex. Li/I2
solvent proportion, chemical composition and preparation techniques
Relevant answer
Answer
You may find the pdf file below useful, hope it helps.
(more details in 1.Intrduction 1.4)
I also find some details of construction of electrolyte in wiki:
"
A separate plate is then made with a thin layer of the iodide electrolyte spread over a conductive sheet, typically platinum metal. The two plates are then joined and sealed together to prevent the electrolyte from leaking. The construction is simple enough that there are hobby kits available to hand-construct them.[14] Although they use a number of "advanced" materials, these are inexpensive compared to the silicon needed for normal cells because they require no expensive manufacturing steps. TiO2, for instance, is already widely used as a paint base.
One of the efficient DSSCs devices uses ruthenium-based molecular dye, e.g. [Ru(4,4'-dicarboxy-2,2'-bipyridine)2(NCS)2] (N3), that is bound to a photoanode via carboxylate moieties. The photoanode consists of 12 μm thick film of transparent 10–20 nm diameter TiO2 nanoparticles covered with a 4 μm thick film of much larger (400 nm diameter) particles that scatter photons back into the transparent film. The excited dye rapidly injects an electron into the TiO2 after light absorption. The injected electron diffuses through the sintered particle network to be collected at the front side transparent conducting oxide (TCO) electrode, while the dye is regenerated via reduction by a redox shuttle, I3/I, dissolved in a solution. Diffusion of the oxidized form of the shuttle to the counter electrode completes the circuit.[15]
"
  • asked a question related to Inorganic Synthesis
Question
7 answers
Educate me please, Why Absorption of Co(III) complex having lower than Co(II) complex. What are important things behind this.
Relevant answer
Answer
OK. prof i agree with you; Changing of charge distribution leads to changing of the chemical environment of the absorbed atom; and the absorption edge will shift in the XANES regime because the core-level energies are changed; every molecule have their distinct charge distributions . However, there are a lot of physical effects evolved in the near-edge region.
  • asked a question related to Inorganic Synthesis
Question
9 answers
I'm wondering if it's possible to make TiO2 as solution for wet chemical route (sol-gel). Is it impossible if I'm going to use acetic acid ? 
 
Second question is, if it's possible to use Ti only or TiCl4? How can I make them to solutions? How can I remove Cl from the solution and my final product ? My final product shouldn't include Cl. It should only be BaTiO3. 
Thank you ☺️!
Relevant answer
Answer
TiO2 is an extremely stable compound. Among the substances typically present in the laboratories only concentrated HF or concentrated H2SO4 will dissolve it. In the second case strong heating (at least 150C) will be needed. Of course, H2SO4 will not work if you need to have Ba in the same solution.
TiCl4 is a good choice even though a bit uncomfortable to use (it releases HCl when contacts with air). You can use a solution in any water-free alcohol. Most of Cl will evaporate in form of HCl during formation and drying of the gel and the remnants can be washed from the precursor afterwards.
The best sources of Ti for the sol-gel synthesis are its alkoxides, but they are really expensive.
  • asked a question related to Inorganic Synthesis
Question
9 answers
Good Evening!
At present I am synthesizing some manganese doped nanoparticles. For that I am in need of MnCl3, but it is not available commercially.
Will anyone can help me to synthesis MnCl3.
I have some formula options. 
2MnO2+ 8HCl = 2MnCl3+4H2O+Cl2, is it possible to get manganese trichloride using this way.
If not. 
KMnO4 + 8HCl = KCl+ MnCl3+4H2O+2Cl2
which one will works.
In the second chemical formula, i want to know how can we get MnCl3 alone as resultant product.
Relevant answer
Answer
Try to understand, MnCl3 is unstable and so you can not keep it as it will release chlorine and will form Mn(II)chloride. For your work follow in this way: Take Mn(II)Cl2 and dissolved it in water and add dilute NaOH solution to precipitate Mn(OH)2 and this will look fleshy white in color.  You can decant the extra liquid and stir this muddy precipitate with a glass rod in air. The colour of the precipitate will change to deep brown. Aerial oxygen will oxidize Mn(II) to Mn(III) hydroxide under alkaline solution and thus the precipitate will change to Mn(III)hydroxide. Under very cold condition add concentrated hydrochloric acid ( ice cooled) into this precipitate to dissolve it to create rown unstable solution of Mn(III) chloride. If you only want to use Mn(III) ion better use manganic(III) acetylacetonate , a nice stable salt of Mn(III) which you can keep in bottle for several days .Hope this will help
  • asked a question related to Inorganic Synthesis
Question
4 answers
I have synthesised copper oxide (I) nanoparticles which shown good photocatalytical properties by oxidation ethylene glycol during 3 hours. But later EG concentration was not changing. Copper +1 reduced to coper 0. Do yu know any photocatalysis which can oxidate EG under visible light during many many days? Thanks  
Relevant answer
Answer
Thanks!
  • asked a question related to Inorganic Synthesis
Question
1 answer
During the AlCl3-catalyzed hydrothermal process, it is possible to form lignin-metal complexation? If possible,  covalent or ionic compounds? and what methods are used for the characterization of these type compounds.I am looking for forward to your reply.Sincerely!
Relevant answer
Answer
Lignin contains many alcoholic and phenolic groups that are capable of binding metals like aluminum(III) through coordinate bonds. These bonds cannot be claimed to be purely ionic or purely covalent. They are coordinate bonds.
  • asked a question related to Inorganic Synthesis
Question
8 answers
Why N-atom is preferred to act as coordinating site than O-atom?
Relevant answer
Answer
because Ru is more "soft"; therefore, N is preffered
  • asked a question related to Inorganic Synthesis
Question
3 answers
I am looking for a metal-organic coordination compound containing 2 atoms of Dy(3+) and one atom of Ti (4+) as a precursor for solution combustion synthesis of dysprosium titanate. 
They may be located both in the core and in the ligands of the molecule.   
Please propose such a compound and method of production thereof in the lab. Many thanks.   
Relevant answer
Answer
Hi,
try searching in CSD (cambridge structural database)
  • asked a question related to Inorganic Synthesis
Question
1 answer
What are the possible ways to synthesize doped SnS3 by simple chemical synthesis without use of hydrothermal reactor. By ways I mean what kind of chemicals. (An acetate or a chloride compound along with the solvent and the capping agent)
  • asked a question related to Inorganic Synthesis
Question
2 answers
I am working on the NVP cathode material for sodium ion batteries. I want to take ICP of that material to get information on chemical composition. I don't know which solvent is suitable for that.
  • asked a question related to Inorganic Synthesis
Question
4 answers
I would like to use 2-bromo pyridine to get 2-cyanopyridine I do need someone  send me the procedure for synthesis.
Relevant answer
Answer
Thank you for your answer, would you please send me the procedure for that.
  • asked a question related to Inorganic Synthesis
Question
4 answers
Measuring phosphorescence of Ru complexes.
Relevant answer
Answer
 chloroform is the best solvent
  • asked a question related to Inorganic Synthesis
Question
3 answers
 I want make quaternary ammonium salts in that we are using benzyl chloride, Final specification benzyl chloride should be less than  0.05% but we are getting 0.1%, how to reduce benzyl chloride content or how to decompose excess benzyl chloride without  disturbing quaternary salts,
Relevant answer
Answer
Thanks for Joseph S Merola and Marius Pelmus
This is product cost itself 90 rs . we are doing this operations means cost will go more than selling price .
  • asked a question related to Inorganic Synthesis
Question
9 answers
Hi everyone,
I am trying to make 200 mM sodium orthovanadate (Na3VO4). According to the protocol I have, I am suppose to adjust pH to 10 with either NaOH or HCl --> solution turns yellow --> Boil for 10 min or until solution turns clear --> cool down --> repeat this 3-5 times until solution doesn't turn yellow with NaOH or HCl anymore.
My problem is that the Na3VO4 solution keeps turning yellow even after 5X I add HCl. It will eventually turn clear when I boil but it will keep turn yellow when I add HCl. The protocol says I need to repeat Boiling-adjusting pH with HCl until the color doesn't change anymore. Could anyone who had the same problem please give me a feedback on this issue? Thank you!
Relevant answer
Answer
Hi Celia,
Try add NaOH first to make it 10 then add drop of HCl, it should turn yellow. Then, comes the boiling step.
  • asked a question related to Inorganic Synthesis
Question
4 answers
In fact I am doing on the synthesis of iron hydroxide using FeNO3 as the precursor and ammonium as precipitating agent. But I faced difficulty during filtration?
Relevant answer
Answer
Maybe you can centrifuge your solution instead ? Usually works for very fine particles
  • asked a question related to Inorganic Synthesis
Question
12 answers
I have tried to find tabular data on the solubilities of various kinds of metal-organic compounds (mainly alkoxane derivatives of transition metals) in organic solvents and I have found mostly fairly old books (back to 1919 and the 1940's). Not that I do not apprecaite old lietrature (our predecessors were frequently more precise and cautious than we are) but since then a lot of new compounds have beed discovered and synthesized. In view of their importance in sol-gel chemistry or in single site catalyst development I presume that tha data base has considerably widened. I hope colleagues workin in this are can share some review articles or the like.
Relevant answer
Answer
Sorry but I can't help you. But I would like to put in evidence that your question is one of most important actual questions: Why a serie of important physical chemical data are available only from papers before Second War? Why people that use and need these data do not publish them? Sure that someone has some data. Mainly of the new compounds......
  • asked a question related to Inorganic Synthesis
Question
5 answers
whenever i add na2so4 in paraphenyldiamine dissolved in dichloromethane the solution is getting green?actually i am synthesising new schiff bases and in my reaction steps i found this problem. 
Relevant answer
Answer
Freshly recrystallized p-phenylenediamine should be colourless. (An aged sample is normally colored). The green colour can be due to the impurities in the diamine. The reaction of a fresh sample p-phenylenediamine with freshly distilled benzaldehyde (commercial benzaldehyde will have benzoic acid impurities) in the appropriate ratio in an alcohol (Methanol or ethanol) should afford the Schiff base as the product. There is no need to use any dehydrating agent including Na2SO4. But in literature there have been claims of making Schiff bases even in water (For details see http://dx.doi.org/10.1016/j.saa.2013.04.026)  which have been proved to be incorrect. 
  • asked a question related to Inorganic Synthesis
Question
5 answers
I want to synthesize  metal oxide (Sodium Nickel Manganese Cobalt  oxide ) from metal acetate precursors. I am synthesizing using Metal acetate as my precursors for sol-gel process. Citric acid is my chelating agent. I was wondering about the optimum pH value i should maintain for the acetate solution to form Gel? Thank you all for your time. Looking forward to know your opinion.
Relevant answer
Answer
Sol-gel process is a subtle balance between hydrolysis and complexation. Complexation is more or less important depending on the nature and on the amount of complexing agent (citric acid in your case), whereas hydrolysis is controlled by pH. Hence pH is at least as important as complexation, and the optimum value depends on the metal alkoxide system you deal with. In the case of silica alkoxides, both acid and basic pH will work, but the result will not be the same (linear species at low pH, highly condensed ones at high pH). For other systems, no gel can form if the pH is not optimal, leading to either precipitates or to molecular complexes instead of gels at the extremes of the pH scale.
Alain
  • asked a question related to Inorganic Synthesis
Question
5 answers
As i know we can treat with oxalyl chloride, SOCl2 to make anhydrous metal salts. Please let me know any other standard procedure.
Relevant answer
Answer
Hi Sudheer,
Could you please let me know what the procedure that you followed to prpare CrBr3 from CrBr3.6H2O? THere is co clear procedure in the literature.
  • asked a question related to Inorganic Synthesis
Question
3 answers
we check the viscosities of commercial products but they stay always stable. the way of preparing the composite may affect this? we use rotary alginate mixer for this purpose or is there some chemicals to help composites maintain its final viscosity?
we also found that the amount of silane used for surface modification affected this much but there is still a problem.
Relevant answer
Answer
Im not after a "secret".. We have been trying to figure out why this change happens over a long period of time. Unlike us, they produce the material in factory conditions. I just wanted to know if we are overlooking a point or doing something wrong.. but thank you, the big idea of checking formulation and structure is what we never thought of and helped a lot.
  • asked a question related to Inorganic Synthesis
Question
11 answers
In the synthesis of Cr(acacBr) {has a brown color} by the bromination of Cr(acac)3 (deep maroon) using NBS, after collecting the crude product, instead of recrystallize it directly I left it in the lab. for 7 days. When I come back to the product its color was green !! I left it brown ! What is the explanation for this observation? does the Cr(acacBr)3 decompose and the Cr3+ reacted with the brome to form CrBr3 {green color} if this is what happened, why did it happened? and what is the mechanism ? 
Relevant answer
Answer
I always caution people not to base too much on color.  It may appear green but not be CrBr3 - do you have any other analysis to suggest that is what you have?  Have you tried recrystallizing to see if you have any of your desired material left? The original Collman paper indicated it should be washed with a number of reagents, some of which will eliminate any excess NBS which is probably your biggest problem.  Finally, that paper also indicated that acetic acid as solvent was important - is that what you used?
  • asked a question related to Inorganic Synthesis
Question
32 answers
Does anyone have a good idea for how to remove a large excess of NaCN from a methanol water solution containing my Fe(II) coordination complex. My complex unfortunately does not ppt but is rather soluble in MeOH/H2O as is the NaCN. I need to add a large excess of NaCN to exchange Cl ligands for CN, I have tried reducing the amount of NaCN used, but then the ligand exchange does not go well. Also my coordination complex is initially formed via a metal templation strategy and when I try other solvents the reaction does not go too well. Any suggestions/ideas would be welcome. I am templating the macrocycle with Fe(II)Cl2 and then exchanging out the Cl's for CN via the addition of an excess of NaCN.
Relevant answer
Answer
Dear Dr. Melanie Pilkington,
may i suggest the use Fe(ClO4)2 instead of chloride salt?and then u can use a stichiometric  amount of cyanide salt instead of excess amount?
  • asked a question related to Inorganic Synthesis
Question
5 answers
I want to increase the crystallinity of a water-insoluble phosphate by use of an autoclave.
In literature the phosphate/water dispersion was kept at 180 °C for one week. Cooling rate was not mentioned.
I wonder if it makes sense to slowly cool down the autoclave or if holding at high temperature is the important step.
I could find out by experiment, but that will take a long time, so any experience would be quite helpful.
Relevant answer
Answer
It depends too much on the system, as sometimes the crystallization occurs on cooling down a solution (cooling down makes the solution become supersaturated), but in solvothermal synthesis anything can happen and I've seen with my eyes crystals growing during heating. 
If your phosphate gets dissolved at 180°C it makes sense to cool down slowly, because new nucleation has to occur and you want only few nuclei, and to grow them slowly.
But if they keep it for 1 week I suppose it stays as a suspension therefore you're trying to improve the crystals you already have, growing them bigger at the expenses of the small ones and/or more ordered.... in this case the cooling rate matters less I think.
Just for fun put 2 autoclaves in the oven, program for slow cooling, but take 1 out after the heating time...
DISCLAIMER: I have no experience with what you're trying to do, I just found the question interesting and sharing my thoughts. I might as well be wrong.
  • asked a question related to Inorganic Synthesis
Question
2 answers
I have a synthetic procedure reported in Russian language. Can someone please translate the text in the highlighted box to me in English? I basically just need to know the procedure for synthesis of NiCl2.2CH3CN from this paper. Would be of great help!
Relevant answer
Answer
Thank you so much Larissa! That helps a lot!
  • asked a question related to Inorganic Synthesis
Question
1 answer
I'm working on the synthesis of S-doped SrTiO3. In many researches i've read there are always the implement of 2-propanol or the mixture of ethylene glycol and citric acid or the mixture of ethanol, ethylene ether, ethylene glycerol, those procedure are chemistry-based methods. So i wonder what is the role of those substance and based on what criteria do we choose the substance and the ratio. Thank you all in advance!!!
Relevant answer
Answer
Hi
One of the most useful application of Citric acid has been employed as a structural modifier. Please, find in attach a site link on Synthesis of single silica nanotubes in the presence of citric acid:
As well as, a paper on A Novel Way to Synthesize Yttrium Aluminum Garnet from
Metal–Inorganic Precursors using citric acid by: Qingmei Lu, Wensheng Dong, Haojing Wang, and Xinkui Wang, published in J. Am. Ceram. Soc., 85 [2] 490–92 (2002) is in attach.
  • asked a question related to Inorganic Synthesis
  • asked a question related to Inorganic Synthesis
Question
3 answers
can anybody tell me the best way for the synthesis of tetrabutyl phosphonium chloride from tetra butyl phosphonium hydroxide.?
Relevant answer
Answer
@michael pach.by treating reactant with hcl.
  • asked a question related to Inorganic Synthesis
Question
3 answers
All Methods of Manufacture H2SO4 Acid?
Relevant answer
Answer
Dear Loutfy,
1- The Contact Process:
makes sulphur dioxide;
convers the sulphur dioxide into sulphur trioxide (the reversible reaction at the heart of the process);
converts the sulphur trioxide into concentrated sulphuric acid.
2- Sulfuric acid is made from dry SO2, O2, N2 gas. The gas comes from combusting elemental sulfur, smelting and roasting sulfide minerals, and decomposing contaminated sulfuric acid catalyst. Sulfur burning is far and away the largest source.
The SO2 in the gas is made into sulfuric acid by (i) catalytically oxidizing it to SO3 then (ii) reacting this SO3 with the H2O(ℓ) component of strong sulfuric acid.
Sulfuric acid is used for making fertilizer, leaching metal ores, refining petroleum, and manufacturing a myriad of products. About 200 million tonnes of sulfuric acid are produced/consumed per year.
3-Burning elemental sulfur
Sixty percent of the world's sulfuric acid is made from elemental sulfur. Virtually, all of this sulfur is the by-product of natural gas and petroleum refining. The first step in making sulfuric acid from elemental sulfur is burning the sulfur with dried air. It entails.
(a) atomizing molten sulfur in a hot furnace and oxidizing the resulting fine droplets with excess dried air
(b) cooling the product SO2, O2, N2 gas in a heat recovery boiler.
The product is ~12 volume% SO2, 9 volume% O2, and 79 volume% N2 gas (420 °C), perfect for subsequent catalytic SO2 oxidation and H2SO4(ℓ) manufacture.
4- About 30% of the world's sulfuric acid is made from the SO2 in smelter and roaster offgases. These gases contain 10-75 volume% SO2. Their SO2 is suitable for making sulfuric acid, but the gases must be cooled, cleaned, diluted, and dried before being sent to acidmaking.
Cooling is usually done in a heat recovery boiler—which cools the gas and recovers its heat as steam. Considerable dust is removed in this heat recovery boiler. Additional dust and unwanted vapors are removed from the gas by subsequent electrostatic precipitation and aqueous scrubbing.
Finally, H2O(g) is removed by (i) condensation and (ii) dehydration with strong sulfuric acid. The gas is then ready for catalytic SO2 oxidation and H2SO4 making
5- Sulfuric acid is used as a catalyst in gasoline, jet fuel, and polymer manufacture. The sulfuric acid catalyst is not consumed, but it becomes ineffective as it absorbs water, hydrocarbons, and other chemicals over time. Its catalytic properties are maintained by bleeding off some of the contaminated “spent” acid and regenerating it to high purity 98% H2SO4() sulfuric acid.
The spent acid bleed is recycled and made into new acid by
(a) decomposing its H2SO4() to SO2, O2, and H2O(g) in a hot (1000 °C), mildly oxidizing furnace
(b) removing dust and condensing water from the decomposition furnace’s offgas
(c) adding air
(d) dehydrating the gas with strong sulfuric acid
(e) catalytically oxidizing the gas’s SO2 to SO3
(f) making new, strong sulfuric acid from (e)’s SO3.
6- SO2-bearing gas must be dry before it goes to catalytic SO2 oxidation. Otherwise, the SO3 made by catalytic oxidation will react with the gas's H2O(g) to form corrosive liquid sulfuric acid in cool flues and heat exchangers, especially during shutdowns.H2Og+H2SO4linstrongacid→H2SO4·H2Olinslightlyweakenedacid
Industrially, the process is carried out in brick-lined stainless steel towers packed with ceramic saddles. Acid descends around the saddles where it meets and reacts with ascending H2O(g)-laden gas.
7- Catalytic oxidation of SO2 to SO3 is a key step in sulfuric acid production. It produces the SO3 required for subsequent H2SO4(ℓ) making. oxidation is always done by passing warm SO2-bearing gas through horizontal beds of V, K, Na, Cs, S, O, SiO2 catalyst. The catalyst promotes rapid SO2 oxidation at temperatures (400-600 °C) where SO2 oxidation is thermodynamically efficient.
Industrially, the oxidation is carried out in a sequence of three to five catalyst beds with gas cooling between beds. Removal of heat from the gas between catalyst beds allows it to leave the last bed at a low temperature (~ 450 °C)—where equilibrium oxidation efficiency is high (98+%).
8- SO3 is a key ingredient in making H2SO4(ℓ). It is produced rapidly and efficiently by oxidizing SO2 to SO3 in a molten V, K, Na, Cs, S, O catalyst film, 400-600 °C. The molten film is supported on a solid, porous silica substrate.
SO2 and O2 dissolve in the molten catalyst. They then react with V, S, O cations to form and release SO3 into the gas. The reactions are rapid at temperatures (400-600 °C) where oxidation is thermodynamically efficient.
The process is carried out industrially in three to five 0.5- to 1-m thick beds of 10- to 25-mm diameter catalyst rings or “star” rings. Gas residence times in each bed are 1.5-2 s.
9- The final step in sulfuric acid manufacture is the production of H2SO4(ℓ) from SO3-bearing gas.
The H2SO4 is made by sending strong sulfuric acid down around ceramic saddles in a packed bed while blowing SO3 gas up through the bed.SO3ginSO3,O2,N2gas+H2Olin98.5mass%H2SO4,1.5mass%H2Osulfuricacid→80-110°CH2SO4linstrengthenedsulfuricacid~99mass%H2SO4
The strengthened acid is mostly diluted and sold. Some is recycled to the dehydration and absorption towers.
Most sulfuric acid plants are double contact plants. They efficiently oxidize their feed SO2 to SO3 and efficiently make the resulting SO3 into H2SO4(ℓ). Single contact plants are simpler and cheaper, but their exit gases contain more SO2.
Hoping this will be helpful,
Rafik
  • asked a question related to Inorganic Synthesis
Question
1 answer
If not, how can you convert ammonium molybdate to sodium molybdate?
Relevant answer
Answer
Not directly, ammonium molybdate, like ammonium metavanadate is only sparingly soluble in dilute sulfuric acid. Add 2M sodium hydroxide to the solid ammonium molybdate warm gently until evolution of ammonia ceases then add your sulphuric acid.
  • asked a question related to Inorganic Synthesis
Question
4 answers
Inorganic synthesis
Relevant answer
Answer
Thank you very much.. 
  • asked a question related to Inorganic Synthesis
Question
2 answers
I want to prepare sulfated zirconia and titania but I only have commercially available zirconia and titania and no precursors. Can I still prepare sulfated versions of zirconia or titania?
Relevant answer
Answer
The two most frequently used approaches are H2SO4 and NH42SO4 (as said above). In the paper linked below, we used decomposition of Zr(SO4)2, but in unpublished work had studied H2SO4 impregnation of ZrO2. This approach gives sulfated zirconia, but didn't work as well for what we were doing. However, different preparation methods give different results for each chemistry investigated. See references in 7.
The same approach is true of TiO2.
  • asked a question related to Inorganic Synthesis
Question
1 answer
I want to know weather PVDF could be used as dopant source for fluorine?  
Relevant answer
Answer
Это должно получиться при обработке гамма излучением образцов после нанесения покрытия. При высокой интенсивности гамма излучения фторированные полимеры подвергаются не контролируемой деструкции и фторируют материалы по различным механизмам, в зависимости от характеристик осколков полимера
  • asked a question related to Inorganic Synthesis
Question
2 answers
As Selenium melting point is 250C, we can't do combustion synthesis. Can anyone suggest us the method of synthesizing SeO2 using Se precursor?
Relevant answer
Answer
Hello,
there is an review on selenium dioxide: Selenium Dioxide: Preparation, Properties, and Use as Oxidizing Agent. G. R. Waitkins, C. W. Clark, Chem. Rev., 1945, 36 (3), pp 235–289
In the laboratory it is oxidized to selenium dioxide by means of strong oxidizing agents such as nitric acid. The usual procedure is to add commercial selenium powder in small amounts to an excess of concentrated nitric acid. The initial reaction is highly exothermic, and clouds of brown fumes of nitrogen dioxide are evolved. The clear solution of selenious acid is fumed to remove excess nitric acid and then evaporated to dryness to dehydrate selenious acid to selenium dioxide. The crude selenium dioxide obtained in this manner is purified readily by sublimation at 317°C. or above to form glistening, white, monoclinic crystals. A product of high purity also can be obtained by direct oxidation of selenium with air or oxygen, using traces of nitrogen oxides as catalysts to promote the reaction. In this method air or oxygen is bubbled into con- centrated nitric acid and then is swept through a glass tube over molten selenium. The selenium dioxide sublimes as it is formed and collects in the cooler end of the tube or in a receiving flask.
With best regards
Marc Birringer
  • asked a question related to Inorganic Synthesis
Question
7 answers
Hello all!
I synthesized UO2-UO3-ZrO2 solid solution using nitrate co-precipitation method. I need to know how much of uranium 4+ I have in my sample in order to perform thermodynamic analysis. 
Thanks beforehand!
Anna.
Relevant answer
Answer
Mr. Paech,
A typical comment from somebody with affiliation a "Company" - what is 'impact' in the science and what is 'not'!
In this context, if we have published a study on "environmental radioanalytical chemistry" based on, for example, "2000" MHz NMR, then no dough, you shall classify our study as an "outstanding contribution" with 'significant impact'. This no dough!
Details about our paper, which not only "impacts", but "contributes", furthermore "significantly" the field of environmental chemistry, first; and second, particularly reflecting in mind the field of radioanalytical chemistry, due to the following, not only one, but a set of reasons:
1. We have reported an analytical protocol based on IR-spectroscopy, which as physical instrumental method provides unique information about the energy profile of the matter. On it base you can conduct a study qualitatively, quantitatively and structurally, furthermore, in gas-phase, solution and in solid-state (incl. analysis of single crystals, polycrystalline samples; glass-state; and amorphous objects). It is applicable to mono- and multicomponent mixtures, operates at minimum sample pretreatment steps, without any chemical transformations, functionalization, purification, isotope dilution and so fourth. For the field of radioanalytical chemistry, the reduced number of chemical treatments is associated with development of more safety for the operators at the first place, protocols. IR-spectroscopy is among the cheapest analytical instrumentation as basic instrumentation and support along with consumables and accessories. This method is widely accessible, thus allowing all elaborations and developments both experimental and theoretical ones, using IR-spectroscopy to be confirmed/rejected and/or further developed within the frame of a large number of independent researchers around the globe. This, generally, is important first to developments of fundamental character. Despite that, it has strong impact to applied elaborations and implementation as well. The novelty here is not the application of IR, but application to non-stoichiometric compositions, which are not trivial objects. Furthermore very similar as chemical content and structures.
2. The second method that we have involved is solid-state MALDI-MS, which as a soft ionization method is little employed for the purposes of environmental radioanalytical chemistry. But: (a) It provides analytical qualitative, quantitative and structural information from low molecular weight analytes to biomacromolecules; including organics, inorganics, metal-organics; (b) The analysis includes in vivo an in vitro screening, analysis of whole organs and bodies. You can study from isolated inorganic radionuclides to monitoring of radionuclides in living systems; (c) It operates at concentration levels from macrocomponents to fmol concentrations (LODs); (d) It allows direct analysis and imaging without any sample pretreatment steps; (e) By MALDI-MS you can study solids (again amorphous, single crystals, polycrystalline and so fourth) and semi-liquid systems; (e) Due to the unique isotope profile of MS shape you can obtain analytical information to all elements of the periodic table; (f) MALDI is applicable to complex multicomponent chemical mixture both homogeneous and heterogeneous due to it high-to-ultrahigh resolving power. In other words you can identify and quantify analytes direct in an environments sample (including biological tissue); (f) In addition to features associated with obtaining of kinetic and exact experimental thermodynamic information, because of the nature of ablation process in MALDI-MS, direct depends on thermodynamic of the corresponding analyte. In this context detail analysis of ionization cross-section and the fragmentation patters provides experimental thermodynamic parameters. There is possible to obtain critical energies of dissociation, energy transfer as well as information about stochastic processes studying the fragmentation nature of precursor ions; (g) In context to point (f) by this method can be studied bulk samples and surfaces, thus yielding to information about corresponding surface interaction processes, reaction kinetics which are highly relevant to the field of environmental analytical chemistry, generally, and not only to the field of environmental radioanalitical chemistry; (h) The basic instrumentation price is higher than this one of IR-instruments, but as instrumental feature MALDI-MS exceeds significantly IR-spectroscopy. As can be seen even only from the written above this method provides analytical chemical information, structural information, kinetics, thermodynamics and so fourth, associated with fundamental and applied aspects to many of the areas of chemistry, physics, biology, medicine. Particularly, describing the chemistry, it is applicable to analytical chemistry, environmental chemistry, geochemistry, food chemistry, physical chemistry, chemical catalysis, organic and metal-organic synthesis, chemistry of polymer, inorganic chemistry, computational quantum chemistry and more.
If for you the involvement of this method in the field of environmental-radioanaltical chemistry is not a "significant impact", then let us pay attention to the methods, discussed in your comments:
(i) XRD methods. No dough XRD based methods are powerful methods, but mainly for structural analysis. However: (a) Are they applicable to all phases - Not!; (b) Are they applicable to quantitative analytical purposes-very difficult-to-not! (c) Are preliminary sample pretreatment and chemical/phase transformation is needed - Yes! (d) Are they applicable to direct multicomponent mixture - difficult-to-impossible; (e) Are they applicable to liquid, semi-liquid and gaseous samples - Not! Are XRD cheap methods - Not! Both as basic prices and consumables. Are they are applicable to large biomacromolecules - yes, but again with sample pretreatment steps and again using not so cheap instrumentation.
(ii) Moessbauer spectroscopy - a magnetic method for analysis operating with XR-source. But, applicable mainly to solids and mainly for qualitative and semi-quantitative purposes. The quantitation, like EPR is often associated with isotope dilution - or, again sample pretreatment steps. Furthermore it is inapplicable to all elements, but to those which are Moessbauer active, and not to all. Applicable to multicomponent isotope mixture or mixtures of one isotope but with different coordination environment?! - Difficult-to-impossible. There is the same problem with chemometrics, typically observed studying quantitative IR-spectra of broad overlapping bands. If the sample contains structurally similar Moessbauer active isotopes, like the samples in our [Ref. 1], then its accuracy significantly decreases in. Furthermore, the concentration LODs are very high 5-10 %. Those values are even higher than LODs of IR-spectroscopy. As concentration LODs, therefore, is fully incomparable with MALDI-MS and any other MS-based method for quantitative analysis. Typical sample quantity? - About 10 (micro)m (also high), furthermore using synchrotron techniques. Please bear in mind that the question to this discussion is relevalt to transdisciplinary areas as well as, including environmental chemistry.
In other words, when given analytical chemical problem, including problem relating environmental analytical chemistry or environmental radioanalytical chemistry, can be solved at a high level of accuracy and precision, providing meaningful scientific information, furthermore applicable to many areas of the science, in parallel by a maximum safety manner, then why this research problem should be solved expensively; not so safety; accompanied with many sample pretreatments, meaning labor costs, furthermore, at a significantly reduced level of scientific information? The question by Ms Shelyug is associated with solid solution where the structures of UO2 and UO3 are presumably kept in this "solution" as a result of precipitation procedure. This can be confirmed qualitatively, quantitatively and structurally within the frame of not more than 15 mins by solid-state IR-accurately, safety (no chemical reactions, chemical functionalization, phase transition, operation at ambient conditions and the like), unambiguously and cheap!. There are only 5 spectra for measurements, in fact.
By the way "papers" are not written to 'help for anyone'! A "scientific publication" reflects scientific achievements; research efforts; individual intellectual contribution to the novelty in the science and/or education; professional competence level of the authors; areas of experience and expertness; conducted research to already granted project/s by third sources of funding, and the like. It 'reflects', do not 'help'! It provides evidence about experience and expertness of academics, which is the most transparent way, ensuring free and loyal competition of academics for employment and research funding by government subsidy in an essencially public sector. Particularly a disribution of research subsidy and positions to the fields of the Higher Education and Research in a public and civil sector, which is not based on a public and transparent publishing process is a source of disloyal competition and corruption (Hochschulgesetz NRW , 9.1.2016, § 36 Einstellungsvoraussetzung en für Hochschullehrerinnen und Hochschullehre (4) 4. für Professorinnen und Professoren an Universitäten darüber hinaus zusätzliche wissenschaftliche Leistungen, die ausschließlich und umfassend im Berufungsverfahren bewertet werden; diese Leistungen werden im Rahmen einer Juniorprofessur, einer Habilitation oder einer Tätigkeit als wissenschaftliche Mitarbeiterin oder als wissenschaftlicher Mitarbeiter an einer Hochschule oder einer außeruniversitären Forschungseinrichtung oder im Rahmen einer wissenschaftlichen Tätigkeit in Wirtschaft, Verwaltung oder in einem anderen gesellschaftlichen Bereich im In- oder Ausland erbracht; Halbsatz 2 gilt nur bei der Berufung in ein erstes Professorenamt).
An example, If X is an author of 100 publications in the field of natural sciences and have received a tenure-truck position here as well as funding by governments subsidy several milions, and in parallel Y in the same scientific area of experience and expertness, as an author of several times more published contributions, furthermore, not only as number (meaning several times more conducted research and efforts or "work") has received a part - time position and negligible funding - this is corruption. Because of the scientific activity of X do not reflects excellences in the experience and expertness in the fields of education and research according above stated Law (Hochschulgesetz NRW , 9.1.2016, § 36(4)), nevertheless the significant number of research grants comparing with Y. In other words, despite the strong finansial support to X, he/she is less competitive comparing with Y in the Labour market of academics. According to the Labour market Laws, however, both X and Y have equal rigths for employment in this sector and funding by governments subsidy. When they have equal rigths in front the Laws, then the employer (Rector in this sector or Director of Research Institute) and the manager of the Funding institutions operating with governments subsidy are obligated to conduct the competition between academics according to the Labour Laws via maximum transparency and objective criteria for this sector (publications, citations, patents, project activity, and so fourth, criteria for attestation which exsist), despite of the general autonomous mechanism of self-organization in those Institutions. Because of the Labour Laws determined by the Parliament stand over any rules of any domestic structures with authonomous mechanizm of organization.
Particular for distribution of academic positions here, and particularly tenure-truck ones to foreigners, where the employment conditions significantly impact the economy (the funding for research is over "de-minimis Beihilfe") thus allowing direct obtaining of citizenship (due to the permanent employment status). Thus the inapplication of the attestation criteria for employment direct arises the question about the 'nature' of the traffic of humans, because of this is a public sector operating with government subsidy. But "Trafficking in human beings is prohibited" (Article 5 (Prohibition of slavery and forced labour) (3), Official Journal of the European Union, 26.10.2012, C 326/391). And thus, this is problem of the Rector/Director as employers to each University/Research Institute, because of those Institutions are independent Juridical Institutions in frond the Laws. When they not apply the attestation criteria to the academics for employment, particularly tenure-track academic positions, which ensure the free competition in this sector of the market, on the base on intelectual achievements, findings, projects and s.o. contributions of the academics, then there is the question about traffic of humans and it "nature" (for foreigners) and/or corruption when the candidates are citizens of the given Country!
In one sentence there is the question: "On which criteria a Rector X of a University Y has decided that exactly candidate Z, having however negligible scientific contributions, furthermore foreigner meaning new citizen with full rights associated with all social services from the site of the Federal Republic of Germany (Germany is one very social Country to German citizens), is particularly prominent for permanet academic position, here?"
Have you understood now what "reflect" the publications of academics, and why they do not "help"?
  • asked a question related to Inorganic Synthesis
Question
7 answers
It is well known that 1,10-phenanthroline (Phen) ligand forms more stable complex with Co(3+) than Co(2+) and Fe(2+) than Fe(3+). This has been attributed to their low spin t2g6 configuration what can be the reason for this enhanced stability how it can be explored computationally?
Relevant answer
Answer
Thanks Priola half part of your answer i have already done by calculating free energies in two oxidation states. yes these  systems have electron delocalization or charge transfer from metal to phen ligand point is how to probe that and how to quantify that the degree of charge transfer is different in two oxidation states.  
  • asked a question related to Inorganic Synthesis
Question
40 answers
any one that work before to prepare hydrazid by reaction of ester and hydrazine hydrate can help me that what is the best Procedure and condition to prepare hydrazid by reaction of ester and hydrazine hydrate  .
i have  acid ethyl ester and   i try before  :
solvent ester in absolute alcohol and then add hydrazine and reflux it
Relevant answer
Answer
Use 5 or 6 equivalent of hydrazine w.r.t. ester and reflux in methanol or ethanol for 6 hrs and then concentrate the solution and keep inside the refrigerator.
  • asked a question related to Inorganic Synthesis
Question
12 answers
Does anyone know how to synthesise pure cobalt carbonate (no basic cobalt carbonate) by precipitation method?
Relevant answer
Answer
I've read a few days ago that by precipitation of an aqueous solution of a cobalt(II) salt with urea at 85oC for 2 hours you can obtain cobalt(II) carbonate. You can find the paper at this link: http://www.ncbi.nlm.nih.gov/pubmed/15350915
  • asked a question related to Inorganic Synthesis
Question
4 answers
We are interested in the synthesis of Pd(COD)I2. Inorganic Syntheses Vol. 13, Drew D. and Doyle D. R., 47-55 gives only a method for the Pt analog. Does anyone own or have access to the book of Hartley, F. R. The chemistry of platinum and palladium: with particular reference to complexes of the elements, 1973, or have experience with the title compound? Thanks.
Relevant answer
Answer
Thank you Saeideh. We have got it now.
  • asked a question related to Inorganic Synthesis
Question
6 answers
How to check from the results of emission or excitation spectrum for metal complexes?
Relevant answer
Answer
Another quick test to differentiate fluorescence from phosphorescence is oxygen quenching.  Assuming your ground state is a singlet, fluorescence won't be quenched by the presence of oxygen, but phosphorescence will.  If you have phosphorescence, which is pretty common in inorganic chromophores, the emission intensity (and lifetime) will decrease in the presence of oxygen.
  • asked a question related to Inorganic Synthesis
Question
1 answer
I was performing the synthesis of ZIF-8 in MeOH. Because I want to add another metal ion in to the framework, Base was used to increase the yield and ensure the proportion close to reactants. I have found some interesting results.
For example, the particle size of Zn:Hmim:NaOH=1:4:2 is much smaller than 1:4:1, which was indicated by the width of XRD peaks. This is easy to understand.
But if TEA was used as the base, the Zn:Hmim:TEA=1:4:2 sample seems to be smaller than Zn:Hmim:NaOH=1:4:2, because the former products(with NaOH) can be filtered by 220 nm Microporous membrane while sample with TEA would block the membrane and have to be collected by centrifugation. 
Therefore, I want to know the difference between NaOH and TEA. 
The synthesis was carried out in the same mode. Solution A contains Hmim and Base; solution B contains anhydrous zinc acetate(for me with some other transition metal salts like cobalt acetate). Both solutions were stirred until all reactants dissolved, and then A was poured into B under stirring. The mixed solution was stirred for 24 hrs at room temperature. Products were collected by filtration or centrifugation and washed with ethanol, dried at 80℃ in vacumm.
XRD shows the product is pure ZIF-8 with high yield(65% for Zn:Hmim:NaOH= 1:4:1 and nearly 100% for 1:4:2).
I would be thankful if someone could share your synthesis of ZIF-8 and its features. For example, maybe DMF is a good solvent.
Relevant answer
Answer
This is a hard question to answer because so many factors could be at play when it comes to synthesis of MOF crystals. Under the assumption that these results you have seen repetitively (i.e., over multiple trials). I have but one question for you.
You have to ask yourself what are all those -OH doing?  Most likely they are terminating the surfaces of the MOF particle (Zn-OH terminating sites) which will actually encourage aggregration between two or more MOF particles. TEA does not generate -OH ions and hence you have smaller particles due to less or no aggregration (aggregration is encouraged by polar ends on a MOF surface).
At least that's what I can think of. May not necessarily be the case
Btw,
What was the yield and purity for your synthesis in TEA in comparison to your NaOH synthesis "XRD shows the product is pure ZIF-8 with high yield(65% for Zn:Hmim:NaOH= 1:4:1 and nearly 100% for 1:4:2)." ?
  • asked a question related to Inorganic Synthesis
Question
6 answers
I was trying to checking the purity of my synthesized complex.
I can't help but to notice there is luminescence in my TLC where the my compound was spotted. But then, the luminescence spot did not rise under DCM and not even hexane an cyclohexane.
Why it did not moved up?
how to seperate the compound from other?
Please advise
Thank you very much
Relevant answer
Answer
If you have a complex that is charged, it probably will not move using DCM alone. Try a 1-10% solution of methanol in DCM. If this helps but the Rf value is still too low, you can try re-crystallization to purify
  • asked a question related to Inorganic Synthesis
Question
8 answers
I want to synthesize HAuCl4 from gold ingot and I need a practical paper.
Relevant answer
Answer
  • asked a question related to Inorganic Synthesis
Question
4 answers
From Axial spectrum, i need to differ both Oh and Sq.Planar complex with supportive values. Can any one help me with related papers.
Relevant answer
Answer
This is a very general question.To answer, one has to have the type of configuration and the crystal field splitting energy. In this case, the number of unpaired electrons can be determined and the expected EPR spectrum will be predicted for the mentioned geometries. .
  • asked a question related to Inorganic Synthesis
Question
3 answers
In following two cases, (i) coordinated with metal complex and (ii) Uncoordinated with metal complex but within crystal lattice.
Relevant answer
Answer
Dear one,
I hope you will get some information about your search , in the file attached.
Good luck
  • asked a question related to Inorganic Synthesis
Question
1 answer
Any references or reviews?
Relevant answer
Answer
Gold, platinum and palladium are particularly effective. A good synthesis technique should lead to Au catalysts that are more active at lower temperatures, but Au is more inclined to sinter at higher (above 350-400C) temperatures.  There are no real problems with these catalysts apart from the usual ones of cost, durability and activity. They also respond to any poisons that might be present in the feed. They need to be placed on suitable support materials at relatively low loadings.
  • asked a question related to Inorganic Synthesis
Question
5 answers
Suggest me a spectrum details in FT-IR, Raman spectrum for perchlorate anion in the metal complex.  
Relevant answer
Answer
From my experience, there is two zones in the IR spectrum to study: near 600 cm-1 and near 1.000-1100 cm-1. When the ClO4 is a free anión (is a counter-ion species) a sharpe and strong band appears near 600 cm-1 and a broad and very strong band at 1100 cm-1. When this species is coordinating to a metal center the first split in two bands or more (depending on the symmetry) as well as the pattern of the last one become more complicated (the broad appearance becomes in a split pattern) because the stretching mode of the vibration Cl-O is not the same for the four bonds in the coordinated species as well as the Td symmetry of the CLO4 species has changed to a minor symmetry.  In addition, if the CLO4 species is coordinating to a metal center there will be appeared in the FAR-IR spectrum the correspondent band(s) due to the metal-O stretching modes.