Catalytic oxygen-scrubber for liquid chromatography

MacCrehan, William A.; Yang, S. D.; Benner, Bruce A.

doi:10.1021/ac00154a021

Cited by 18 publications

(5 citation statements)

References 12 publications

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“…Early work using acetonitrile/water eluents employed a zinc oxygen scrubber column (39). However this scrubber has several drawbacks (44) including the production of troublesome zinc particles as well as the need for frequent replacement. For later work, we used a platinum oxygen scrubber in conjunction with methanolic eluents.…”

Section: Methodsmentioning

confidence: 99%

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Determination of nitro-polynuclear aromatic hydrocarbons in air and diesel particulate matter using liquid chromatography with electrochemical and fluorescence detection

MacCrehan¹,

May²,

Yang³

et al. 1988

Anal. Chem.

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102

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Three different approaches to the liquid chromatographic detection of nitro polynuclear aromatic hydrocarbons In air and diesel particulate extracts are presented, based on differential pulse (LCDPD) and amperometrlc (LCEC) electrochemical detection and fluorescence detection following online reduction to the amine (LCFI). The particulate extractlon/fractlonatlon procedure for each detection approach Is discussed. The operational advantages of oxygen removal with a platinum oxygen scrubber (aM three types of detection), the use of modulated pulse detection, and wavelength-programmed fluorescence detection are explored. 1-NKropyrene Is determined In Standard Reference Material (SRM) 1650 diesel particulate matter and In several other "round robin" samples by aH three methods. Results are compared to those obtained by other techniques (gas chromatography/mass spectrometry) and by other laboratories (LCFI). Additionally, 2-nltrofluorene, 9-nHroanthracene, 7-nltrobenz[a ]anthracene, and 6-nHrobenzo[a]pyrene are determined In SRM 1650 by LCFI. The detection limits for 1-nltropyrene (expressed as plcograms) are 5200 (LCDPD), 60 (LCEC), and 10 (LCFI).

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Section: Methodsmentioning

confidence: 99%

“…For later work, we used a platinum oxygen scrubber in conjunction with methanolic eluents. This scrubber catalyses the reduction of the dissolved oxygen by methanol added to the mobile phase (44). The oxygen scrubber column was a 15 X 0.46 cm bed packed with 10% platinum-on-alumina catalyst (Alfa Products, Danvers, MA).…”

Section: Methodsmentioning

confidence: 99%

Determination of nitro-polynuclear aromatic hydrocarbons in air and diesel particulate matter using liquid chromatography with electrochemical and fluorescence detection

MacCrehan¹,

May²,

Yang³

et al. 1988

Anal. Chem.

Self Cite

102

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“…Note that the calibration curves do not all provide the same response for the three calibrants. The peak signal is a function of the release of the explosive vapors from the swipe in the heated zone of the sampling port . The 0.1% SRM material provides the most response per nanogram of TNT, despite being incorporated into the C 18 matrix.…”

Section: Resultsmentioning

confidence: 99%

A NIST Standard Reference Material (SRM) to Support the Detection of Trace Explosives

MacCrehan

2009

Anal. Chem.

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SRM 2905 Trace Particulate Explosives was developed to simulate the residues produced by handling plastic and military explosives. A series of nine candidate materials were prepared by coating chromatographic supports with either Composition C-4 (containing RDX (hexahydro-1,3,5-trinitro-1,3,5-Triazine) and HMX (octahydro-1,3,5,7-tetranitro-1,3,5,7-Tetrazocine)) or TNT (2,4,6-trinitrotoluene). Criteria for selection of the best material for the SRM included: coating efficiency, extractability with organic solvents, thermal storage stability, consistency of the particle size with fingerprint residues, and suitability for calibration of trace explosives detectors. The final base material selected for the SRM was octadecylsilane-modified silica (C(18)) with a nominal 20-30 microm particle size. Four materials comprise the SRM, with two nominal concentrations of explosive, 0.01% and 0.1% (mass fraction) for both C-4 and TNT, respectively. The final certified concentrations were determined by liquid chromatography (LC) with ultraviolet absorbance detection (LC/UV) and a liquid chromatography with mass spectrometric (LC/MS) method using negative ion atmospheric pressure ionization (APCI(-)) with an acetate ionization additive that improves quantitation. The SRM was tested on a table-top field explosives detector based ion mobility spectrometry (IMS).

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“…In this work, electrochemical activated glassy carbon electrodes were employed to the electroanalysis of nitro polycyclic aromatic hydrocarbons. 1-Nitropyrene has become a benchmark compound for both analytical and mutagenicity studies, since it has been found to be responsible for 3±23 % of the mutagenicity of the air and diesel particulate extracts [4]. So, the preconcentration and determination of nitropyrene as a test sample at pretreated glassy carbon electrode were investigated in detail.…”

Section: Introductionmentioning

confidence: 99%

Preconcentration and Electrochemical Determination of Nitropyrene at Electrochemically Activated Glassy Carbon Electrodes

Song¹,

Lee²,

Shiu³

2000

Electroanalysis

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Polycyclic aromatic hydrocarbons substituted with one or more nitro-groups (nitro-PAHs) have been proven to be carcinogenic. This work provides the ®rst report on the electroanalysis of nitro-PAHs using chemically modi®ed electrodes. A representative nitro-PAH species, namely nitropyrene was readily extracted onto electrochemically pretreated glassy carbon electrodes (pGCE) from methanol solution. The nitropyrene species adsorbed on pGCE were reduced electrochemically to aminopyrene in a 6-electron process in 0.5 M H 2 SO 4 . Both nitropyrene and aminopyrene were found to adsorb strongly on pGCE. Experimental results showed that the peak current resulting from nitropyrene reduction was proportional to the concentration in their methanol solution for a wide dynamic range from 5 to 1500 ng/mL with a large slope of 0.0864 A L g 71 and a correlation coef®cient of 0.999. The preconcentration and determination conditions, as well as possible interference from other PAH species, were investigated. Possible application in the determination of nitropyrene in air particulate was evaluated.

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Catalytic oxygen-scrubber for liquid chromatography

Cited by 18 publications

References 12 publications

Determination of nitro-polynuclear aromatic hydrocarbons in air and diesel particulate matter using liquid chromatography with electrochemical and fluorescence detection

Determination of nitro-polynuclear aromatic hydrocarbons in air and diesel particulate matter using liquid chromatography with electrochemical and fluorescence detection

A NIST Standard Reference Material (SRM) to Support the Detection of Trace Explosives

Preconcentration and Electrochemical Determination of Nitropyrene at Electrochemically Activated Glassy Carbon Electrodes

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