What would be the fastest and easiest way to titrate a LiHMDS solution?

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Bruce Levison

4-Phenylbenzylidene benzylamine: A new and convenient reagent for the titration of solutions of lithium alkyls and metal amides Journal of Organometallic Chemistry Volume 448, Issues 1–2, 20 April 1993, Pages 1-3

4-(Phenylazo)diphenylamine (PDA): a universal indicator for the colorimetric titration of strong bases, Lewis acids, and hydride reducing agents Tetrahedron Letters Volume 56, Issue 23, 3 June 2015, Pages 3674–3678

http://ac.els-cdn.com/0022328X9380058J/1-s2.0-0022328X9380058J-main.pdf?_tid=be84cd18-0a75-11e7-b3bc-00000aacb362&acdnat=1489688828_8ba28f6a4b47a08bab3f0f7ae6793759

http://ac.els-cdn.com/S0040403915003391/1-s2.0-S0040403915003391-main.pdf?_tid=d5e567ce-0a75-11e7-8bd7-00000aacb360&acdnat=1489688867_6b229fa228a65f0d989cfc0f6df1ab68

Andrei Rogoza

Easiest way is cooling in fridge below 0oC - LiHDMS crystallizes perfectly from concentrated hexane solution as ~100% pure compound. After cold filtering in inert atmosphere, crystals are suitable for any manupulation.

1H NMR with pre-weighted standard (TMS of HMDS) allow to quantify LiHMDS in solution

Ajeesh Kumar

IH NMR assay will help to quantify the same