Chromatographic Separation Method for the Simulant Mixture of TriisopropylPhosphite and Bis(2-Ethylhexyl) Hydrogen Phosphite

摘要

A simulant mixture has been devised for the Bigeye Fill Close Facility. Theability to analyze for the proposed simulant mixture has called upon an assay analysis for purity. The purity evaluation of triisopropyl phosphite (TIP), bis-(2-ethylhexyl) hydrogen phosphite (BIS), and mixtures of these two compounds is to be performed with gas chromatographic (GC) separation using thermal conductivity detection (TCD). A natural impurity within the TIP is that of diisopropyl hydrogen phosphite (DIP) that could yield an error in the purity results if coelution with TIP occurs. Using a glovebox, investigators transferred samples of TIP, BIS, and DIP to sample vials under a nitrogen blanket. Additional samples were transferred to tubes in a similar manner for evaluation by Fourier Transform (FT) NMR. The primary method of evaluation was to make individual injections of these chemicals, along with mixture injections of TIP/DIP and TIP/BIS to obtain suitable chromatographic separations of the components. The methods' development involved evaluating instrumental parameters using megabore GC columns.