Dear Abdul Sattar the fact that you isolated crystalline solid already indicates that you obtained the desired salts. The easiest way to determine their purity would be an elemental analysis. You can of course also run NMR spectra ofthe two salts. Cited below are some references which are available on RG:

Article Ethylenediammonium dichloride

Article Ethylenediammonium dichloride

Try Elemental Analysis

Dear Abdul Sattar the fact that you isolated crystalline solid already indicates that you obtained the desired salts. The easiest way to determine their purity would be an elemental analysis. You can of course also run NMR spectra ofthe two salts. Cited below are some references which are available on RG:

Article Ethylenediammonium dichloride

Article Ethylenediammonium dichloride

Instead of asking others for everything, you should try to learn on your own and in that process you will become an expert, because in that process you learn many other things in detail if you devote more time. This habit of asking others for everything will make one less knowledgeable at the end of the day.

First of all, check the method you used. Did you use dry conditions, did you use anhydrous HCl gas freshly prepared and passed through a drying chamber before pubbling. If not, you should know what are the methods at your disposal to make the desired compound. When you take all these precautions, you will get only the pure product. This is highly hygroscopic in nature. After making anything, unless they are highly ionic with high melting point, you can ascertain the purity simple looking to mp. If it shows sharp mp, it has to be pure compounds, if it melts over a range or showing two or more melting zones, it is a mixture. Then look for NH stretching in IR and take NMR and eventually elemental analysis. There is no need to go for xrd. If you follow simple methodology, you can check yourself without asking others.

Start this method for your next experiment and in a year you will be an expert in synthesis.

Good Luck

Balakrishna

XRD is of little help if you don’t know what the crystal lattice looks like. Elemental analysis is your best option; I would recrystallize until the analysis is acceptable.

Dear Balakrishna Maravanji your answer is indeed very useful but not very polite. Isn't it the purpose of RG that young researchers ask questions to seek help from experienced researchers?

Dear Abdul Sattar in terms of content I fully agree with the answers given by Balakrishna Maravanji and James Demers. Measuring XRD spectra is like "taking a sledgehammer to crack a nut"! In your case, traditional characterization methods like elemental analysis, IR and melting point are more appropriate and informative.

I would think that both these salts are long reported in the literature and are well characterized which means that melting points and spectra are reported for both compounds. To insure complete dihalide formation the molar amount of acid must be greater than two fold. A Beilstein flame test on the products would be qualitatively informative. H-NMR for both when pure should integrate for only five protons and D2O exchange should reduce that to two. Normally organic ammonium chlorides are are prepared by adding the amine to 6N anhyrous HCl in isopropanol. Ammonium idides are more difficult as they tend to be hydroscopic and I have prepared very few of them. But check the literature.

Dear Abdul Sattar and Jack M Hinkley I would like to add that both salts are also commercially available from various sources.

Dear Frank T. Edelmann, I really appreciate your comments for helping me out. I will follow the protocol in light of your opinion. Thank you Sir!

Dear Abdul Sattar you're very welcome! Good luck! 😊

Dear Balakrishna Maravanji Sir, I thank your for the advice and also for the guidance that you give to improve synthesis procedures. Actually, I have a background in electrical engineering and shifted to the material science related to photovoltaic systems. I am eager to learn general synthesis techniques and methodology. Can you please suggest me any book covering overall topics related to organic or inorganic synthesis techniques?

Frank T. Edelman, I know. However, that was not my understanding of the intent of the question. jmh

Dear Abdul Satter

I recommend that you discuss a knowlegable synthatic chemist face to face your desire to learn synthetic techniques and methodology. This person should be able to give guidance on where to start. There is a lot to learn. jmh

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