Matrix-assisted ionization (MAI)-mass spectrometry (MS) eliminates the need for high voltage, a heat source, lasers, and compressed gases in the ionization process and uses minimal solvents in sample preparation, thus making MAI ideal for field-portable mass spectrometers. The broad applicability of MAI is demonstrated by simple, rapid, and robust positive and negative detection mode analyses of low and high mass compounds including some pesticides, dyes, drugs, lipids, and proteins (186 Da to 8.5 kDa) from various materials including urine, biological tissue sections, paper, and plant material on a low pumping capacity, single-quadrupole mass spectrometer. Different sample introduction methods are applicable, including the use of a pipet tip or glass melting point tube, allowing integration of sample preparation with sample introduction for increased analytical utility and ease of operation, even when sampling directly from surfaces.
Cisplatin, (NH3)2PtCl2, has been known as a successful metal-based anticancer drug for more than half a century. Its analogue, Argplatin, arginine-linked cisplatin, (Arg)PtCl2, is being investigated because it exhibits reactivity...
Deposition rate is known to affect the relative stability of vapor-deposited glasses; slower rates give more stable materials due to enhanced mobility at the free surface of the film. Here we show that the deposition rate can affect both the thermodynamic and kinetic stabilities of N,N-bis(3-methylphenyl)-N,N-diphenylbenzidine (TPD) and N,N-di-[(1-naphthyl)-N,N-diphenyl]-1,1'-biphenyl)-4,4'-diamine (NPD) glasses used as hole transport layers for organic light emitting diodes (OLEDs). A simple, low-vacuum glass sublimation apparatus and a high vacuum deposition chamber were used to deposit the glass. 50 μm thick films were deposited in the sublimation apparatus and characterized by differential scanning calorimetry while 75 nm thick films were prepared in the high vacuum chamber and studied by hot-stage spectroscopic ellipsometry (SE). The thermodynamic stability from both preparation chambers was consistent and showed that the fictive temperature (T) was more than 30 K lower than the conventional glass transition temperature (T) at the slowest deposition rates. The kinetic stability, measured as the onset temperature (T) where the glass begins to transform into the supercooled liquid, was 16-17 K greater than T at the slowest rates. T was systematically lower for the thin films characterized by SE and was attributed to the thickness dependent transformation of the glass into the supercooled liquid. These results show the first calorimetric characterization of the stability of glasses for OLED applications made by vapor deposition and the first direct comparison of deposition apparatuses as a function of the deposition rate. The ease of fabrication will create an opportunity for others to study the effect of deposition conditions on glass stability.
Modifications to a Paul-type quadrupole ion trap mass spectrometer providing optical access to the trapped ion cloud as well as hardware and software for coupling to a table-top IR optical parametric oscillator laser (OPO) are detailed. Critical experimental parameters for infrared multiple photon dissociation (IRMPD) on this instrument are characterized. IRMPD action spectra, collected in the hydrogen-stretching region with this instrument, complemented by spectra in the IR fingerprint region acquired at the FELIX facility, are employed to characterize the structures of the protonated forms of 2-thiouridine, [sUrd+H], and 4-thiouridine, [sUrd+H]. The measured spectra are compared with predicted linear IR spectra calculated at the B3LYP/6-311+G(d,p) level of theory to determine the conformers populated in the experiments. This comparison indicates that thiation at the 2- or 4-positions shifts the protonation preference between the 2,4-H tautomer and 4-protonation in opposite directions versus canonical uridine, which displays a roughly equal preference for the 2,4-H tautomer and O4 protonation. As found for canonical uridine, protonation leads to a mixture of conformers exhibiting C2'-endo and C3'-endo sugar puckering with an anti nucleobase orientation being populated for both 2- and 4-thiated uridine. Graphical Abstract ᅟ.
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