Integrated Lab-in-Syringe Platform Incorporating a Membraneless Gas–Liquid Separator for Automatic Cold Vapor Atomic Absorption Spectrometry

Abstract

This manuscript reports the proof-of-concept of a novel integrated lab-in-syringe/gas-liquid separation (LIS/GLS) batch-flow system based on a programmable flow for automatic cold vapor atomic absorption spectrometric assays. Homogeneous mixing of metered volumes of sample and reagent solutions drawn up in a sandwich-type mode along with in situ vapor generation are accomplished inside the microsyringe in a closed manner, while the separation of vapor species is achieved via the membraneless GLS located at the top of the syringe's valve in the upright position. The potentials of the proposed manifold were demonstrated for trace inorganic mercury determination in drinking waters and seawater. For a 3.0 mL sample, the limit of detection and repeatability (RSD) were found to be 0.03 μg L(-1) Hg(II) and 3.1% (at the 2.0 μg L(-1) concentration level), respectively, with a dynamic range extending up to 10.0 μg L(-1). The proposed system fulfills the requirements of US-EPA, WHO, and EU Council Directives for measurements of the maximum allowed concentrations of inorganic mercury in drinking water.

Automated headspace single-drop microextraction via a lab-in-syringe platform for mercury electrothermal atomic absorption spectrometric determination after in situ vapor generation

“…The sample solution and the reducing agent were aspirated subsequently into the SB by means of the SV in a similar way as in lab-on-valve systems. 14 A prominent advantage of the LIS-HS device is the fact that reduced pressure (<0.2 atm) into the SB can be easily produced by downwards movement of the piston while SV valve is in a plugged port (Fig. 1, port 4).…”

“…Similar methodology was later reported for spectrophotometric assays of copper and aluminum in syringe dispersive liquid-liquid microextraction 12,13 and for automatic cold vapor atomic absorption spectrometric determination of mercury using a novel integrated lab-in-syringe/gas-liquid separation (LIS/GLS) programmable batch-ow system. 14 An inherent advantage of LIS systems is the fact that the syringe pump is an entirely closed reaction vessel with great potential for accommodation of vapor generation approaches.…”

Automatic In-Syringe Dispersive Microsolid Phase Extraction Using Magnetic Metal–Organic Frameworks

“…To date, just one approach for automatic magnetic D-µ-SPE has been described, which is based on the use of dissolvable Fe 3 O 4 -layered double hydroxide core-shell microspheres as sorbent, and a dedicated autosampler as automation tool. 21 We report, in the present work, a novel approach for the automation of D-µ-SPE using magnetic materials based on the recently described lab-in-syringe concept, [22][23][24][25] which allows to fully benefit of the properties of the sorbent. Using this approach, the implementation of magnetic MOFs for automatic SPE has been carried out for the first time.…”

“…We report, in the present work, a novel approach for the automation of D-μ-SPE using magnetic materials based on the recently described lab-in-syringe concept, − which allows the full benefit of the properties of the sorbent. Using this approach, the implementation of magnetic MOFs for automatic SPE has been carried out for the first time.…”

Fully Automatic In-Syringe Magnetic Stirring-Assisted Dispersive Liquid–Liquid Microextraction Hyphenated to High-Temperature Torch Integrated Sample Introduction System-Inductively Coupled Plasma Spectrometer with Direct Injection of the Organic Phase

“…While there has been significant work harnessing flow-based approaches (mostly flow injection and sequential injection) for automated liquid–liquid extraction of metal species, ,,− with potential implementation in microfluidic devices, ,, prior to online atomic spectrometric detection, reviewed elsewhere, ,− just a few papers report on employing LIS, whose versatility has not been fully explored yet. LIS for metal assays has been merely coupled to atomic absorption spectrometric measurements, namely, mercury microextraction and cold vapor atomic absorption spectroscopy , and more recently to nondispersive liquid phase extraction of silver followed by GFAAS, yet studies concerning online dispersive liquid–liquid microextraction (DLLME) as a front-end microextraction approach to multielemental ICP OES/MS are still missing.…”