I am currently working on the degradation study of harmful organic contaminants present in the in the industrial effluents with the help of advanced oxidation processes. The color solution of the sample changes as soon as the reagents are added into the solution , which may due to the formation of intermediates. I want to know the best and reliable laboratory equipments/techniques which will help in identifying and categorize these intermediates formed as by product.
Naveen Kumar Chaturvedi this is the most important question during the degradation of organic matter over the advance oxidation process. to investigate the intermediate product you can use HPLC/MS. scavenger tests can help you to explain the mechanism.
Dear Nk Choudhry,
Apropos to your Qs you can refer this following DOI for further reading.
(https://doi.org/10.1007/s40710-018-0284-9)
If intermediates cannot be trapped, or have a short life, I suggest ESI-MS of the solution or the model system at a given reaction time. You may even use a mixing system (two syringes connected to Tee with the exit going to the MS source) for examining fast reactions.
I don't know whether we have a real time or insitu HPLC-MS in the markets today. the instrument that can give real time monitoring would do the job best.
Aldo Okullo Apita the reaction may be followed in real time by ESI if not too fast, let say a few minutes minimum. If too fast, it is possible to try the simple online mixing, as I described yesterday.
In many AOP processes there are doubts about the reaction mechanisms and the routes that they follow, I think that with the ESI-MS, I could give an answer to the degradation routes that some AOPs follow.
I want to thankyou all for giving valuable comments and suggestions.
Looking back at the initial question summarized as "identifying and categorize these intermediates formed as by product" and reading the answers, it seems that there is a lack of precise definition of "intermediate". First, byproducts are not directly intermediates, they are rather products from undesired reaction(s), or side-products. Stable intermediates in a reaction maybe observed at low conversion time, when the reaction is not complete. They may persist in small quantities depending in the treatment of the reaction products. Degradation products may appear because the expected product is suffering a secondary reaction under the experimental conditions. "Intermediates" may also mean unstable / transient species which occurs during the process, but cannot be easily observed or trapped. In the latter case, ESI MS may be tried, at low reaction times using fast mixing of reactants.
LC-Ms for sure
please see this article:
https://doi.org/10.2166/wst.2016.339
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