Mitigation of signal suppression caused by the use of trifluoroacetic acid in liquid chromatography mobile phases during liquid chromatography/mass spectrometry analysis via post‐column addition of ammonium hydroxide

A method has been developed to reduce the mass spectrometric ion signal suppression associated with the use of TFA as an additive in LC mobile phases. Through post‐column infusion of diluted NH₄OH solution to LC eluents, the ammonium ion introduced causes the neutral analyte‐TFA ion pair to dissociate which consequently releases the protonated analyte as free ions into the gas phase (through regular electrospray ionization mechanisms). An ion signal improvement from 1.2 to 20 times for a variety of compounds had been achieved through the application of this method. The molar ratios of NH₄OH:TFA which result in a reduction of signal suppression were determined to be between 0.5:1 and 50:1. In addition, it was shown that this NH₄OH infusion method could reduce the level of doubly‐charged species and the product ions formed via in‐source collision. The use of diluted NH₄OH solution is favorable since it is compatible with mass spectrometry analysis, and it is applicable in both positive and negative‐ion generation mode. Copyright © 2012 John Wiley & Sons, Ltd.     

Sub‐millisecond transient vertical chevron formation during the electroclinic effect in the smectic A∗ phase

X‐ray diffraction studies are carried out in order to probe the smectic layer structure in liquid crystal devices filled with FLC mixture SCE8 and AFLC mixture CS4001, at a temperature just above the SmA?–SmC? phase transtion. The data gathered are time‐resolved in synchronization with a bipolar voltage pulse applied across the device. The layers are observed to move dynamically and reversibly with voltage application and removal, giving evidence for temporary vertical chevron formation due to the electroclinic effect on a timescale consistent with this phenomenon.