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1.
Metrologia ; 57(2)2020.
Artigo em Inglês | MEDLINE | ID: mdl-38487595

RESUMO

Despite ubiquitous implementation of the quartz crystal microbalance (QCM) for measuring thin film thickness throughout industry and academia, a direct link to the SI (International System of Units) does not exist. Confidence in QCM measurements relies on over a half-a-century of academic and industrial research used to understand the resonant frequency change due to loading mass onto a quartz crystal. Here, we use before and after gravimetric mass measurements, linked directly to the SI, to measure mass change. A custom vacuum metal deposition system is used to deposit gold films of various masses onto a series of quartz crystals while the mass dependent frequency change is monitored in real time. The gravimetric (known) mass changes are compared to three analytical methods (frequency, time and energy) used to convert resonant frequency shifts to mass changes, none of which rely on the material properties of the deposited material. Additionally, we evaluate the reversible and irreversible contributions to mass change from the loading into, and removal from, the vacuum environment. We find the "energy-based" method for frequency to mass conversion has the best accuracy over the longest range, at 0.36 % to > 1 mg. Only for mass changes below 100 µg are deviations > 2 % observed. A complete uncertainty budget is provided.

2.
Lab Chip ; 15(7): 1748-58, 2015 Apr 07.
Artigo em Inglês | MEDLINE | ID: mdl-25673367

RESUMO

This paper reports a unique GC-on-chip module comprising a monolithically integrated semi-packed micro separation column (µSC) and a highly sensitive micro helium discharge photoionization detector (µDPID). While semi-packed µSC with atomic layer deposited (ALD) alumina as a stationary phase provides high separation performance, the µDPID implemented for the first time in a silicon-glass architecture inherits the desirable features of being universal, non-destructive, low power consumption (1.4 mW), and responsive. The integrated chip is 1.5 cm × 3 cm in size and requires a two-mask fabrication process. Monolithic integration alleviates the need for transfer lines between the column and the detector which improves the performance of the individual components with overall reduced fabrication and implementation costs. The chip is capable of operating under the isothermal as well as temperature and flow programming conditions to achieve rapid chromatographic analysis. The chip performance was investigated with two samples: 1) a multi-analyte gas mixture consisting of eight compounds ranging from 98 °C to 174 °C in boiling point and 2) a mixture containing higher alkanes (C9-C12). Our experiments indicate that the chip is capable of providing rapid chromatographic separation and detection of these compounds (<1 min) through the optimization of flow and temperature programming conditions. The GC-on-chip demonstrated a minimum detection limit of ~10 pg which is on a par with the widely used destructive flame ionization detector (FID).


Assuntos
Cromatografia Gasosa/instrumentação , Alcanos/análise , Desenho de Equipamento , Gases/análise , Limite de Detecção , Técnicas Analíticas Microfluídicas
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