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At least 685 records · Page 38
All sourcesNASA NTRSDOE OSTI
DOE OSTI2017

High-resolution ultrahigh-pressure long column reversed-phase liquid chromatography for top-down proteomics

We report development of an approach providing high-resolution RPLC of proteins and its utility for mass spectrometry-based top-down proteomics. A chromatographic peak capacity of ~450 was achieved for proteins and large polypeptides having MWs up to 43 kDa in the context of proteomics applications. RPLC column lengths from 20 to 200 cm, particle sizes from 1.5 to 5 m, bonding alkyl chains from C1 to C2, C4, C8, and C18, and particle surface structures that spanned porous, superficially porous (porous shell, core-shell), and nonporous were investigated at pressures up to14K psi. Column length was found as the most important factor for >20 kDa proteins in gradient RPLC, and shortening column length degraded RPLC resolution and sensitivity regardless of the size and surface structure of the packing particles used. The alkyl chains bonded to the silica particle surface significantly affected the RPLC recovery and efficiency, and short alkyl C1-C4 phases provided higher sensitivity and resolution than C8 and C18 phases. Long gradient separations (e.g., >10 hours) with long columns (e.g., 100 cm) were particularly effective in conjunction with use of high accuracy mass spectrometers (e.g., the Orbitrap Elite) for top-down proteomics with improved proteoform coverage by allowing multiple HCD, CID, and ETD dissociation modes. It was also found that HCD produced small fragments useful for proteoform identification, while low energy CID and ETD often complemented HCD by providing large fragments.

columns and stationary phases↗
DOE OSTI2015

High voltage LIB cathodes enabled by salt-reinforced liquid electrolytes

We report on electrochemical properties of Li/Li 1.2 Ni 0.15 Co 0.1 Mn 0.55 O 2 secondary batteries in electrolytes designed to stabilize electrodeposition of lithium. Ethylene carbonate (EC): dimethyl carbonate (DMC) containing a LiPF6/LiF salt blend stabilizes lithium electrodeposition and enables Li/Li 1.2 Ni 0.15 Co 0.1 Mn 0.55 O 2 batteries with a high discharge capacity of 270 mAh·g - 1 at 0.05 mA cm - 2 . Cells containing the LiF-reinforced electrolytes also exhibit excellent capacity retention over 500 cycles with Columbic efficiencies approaching 100%. Post-mortem SEM analysis of the lithium anode shows more compact deposition in the presence of the LiF salt additive, while XPS depth profile analysis of cathodes show a more uniform distribution of Mn over the first 180 nm from the electrode/electrolyte interface. The results imply that LiF reinforced electrolytes simultaneously facilitate stable lithium electrodeposition and reduce Mn dissolution.

25 ENERGY STORAGE↗