danaH Posted June 10, 2011 Posted June 10, 2011 Hey,,, someone here worked with NICKEL CHLORIDE HEXAHYDRATE? i have in the lab a big stock of it, but i wanna work with the dry nickel chloride! it can be dried good enough on high vacuum and heat to work with moisture sensitive ligands? or i should order dried one?
hypervalent_iodine Posted June 10, 2011 Posted June 10, 2011 Just heating it won't do much. I think if you heat it in conjunction with some like thionyl chloride, you should get the anhydrous stuff, SO2 and a bunch of HCl. The product will be yellow.
danaH Posted June 10, 2011 Author Posted June 10, 2011 ohh,,,cool,,,i just found this book now: http://onlinelibrary.wiley.com/doi/10.1002/9780470132593.ch80/summary;jsessionid=3D3BD722D2E786D787F1E14197938DC0.d03t01 i dont have access to it,,, maybe we have it at the library,,, thank you again:)
mississippichem Posted June 10, 2011 Posted June 10, 2011 Just heating it won't do much. I think if you heat it in conjunction with some like thionyl chloride, you should get the anhydrous stuff, SO2 and a bunch of HCl. The product will be yellow. Having done this myself, I second that opinion.
danaH Posted June 10, 2011 Author Posted June 10, 2011 ohhh great,,,!! i will save some money for my supervisor by not ordering the anhydrous this way and i will have more metal to try my experiments with! cool!!
hypervalent_iodine Posted June 10, 2011 Posted June 10, 2011 As a side note, I use thionyl chloride a fair bit in my work and having seen what it does to disposable syringe needles, I would strongly recommend against using it with a syringe that is not disposable. It corrodes metal rather quickly. And don't make the mistake I once did and make sure you screw the lid on nice and tight. Cleaning a corrosives cabinet filled with thionyl chloride and HCl isn't exactly fun.
danaH Posted June 12, 2011 Author Posted June 12, 2011 i just saw the message after i started the reaction it goes really nice...i need to distill in one hour the thionyl chloride and put the nickel in a desiccator ... soon i will have about 10 grams of nickel chloride,,,thank you
danaH Posted June 14, 2011 Author Posted June 14, 2011 the nickel looks brown and not yellow....you think it is ok? i will enter it to the glove-box after drying on high-vacuum,,, and i will take NMR,,,,hope it is ok!
hypervalent_iodine Posted June 14, 2011 Posted June 14, 2011 I try not to base my assessment off of colour and appearance as it can lead you astray sometimes, but it sounds as though it would be okay. Best to check the NMR
danaH Posted June 14, 2011 Author Posted June 14, 2011 yea...i know color might be misleading,,,,but it is so frustrating when u get something different from what is reported thank you again !
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