Wall-coated open-tubular column chromatography on an organo–clay stationary phase

Bruno, Thomas J.; Lewandowska, Aneta; Tsvetkov, Faina; Miller, Keith E.; Hanley, H. J. M.

doi:10.1016/s0021-9673(02)01124-x

Cited by 15 publications

(6 citation statements)

References 16 publications

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“…As the ignitable liquid vaporizes, it is possible for partitioning to take place with the substrate; interactions with the substrate may cause some molecules of the ignitable liquid to be retained more strongly than others. Examination of enthalpy of adsorption measurements of n-alkanes (the most extensively studied family of compounds) shows that many surfaces will interact strongly [ 37 ]. While the effect of intermolecular interaction has not been fully studied for typical arson substrates, we point out that the interaction is a surface phenomenon.…”

Section: Ignitable Liquidsmentioning

confidence: 99%

Weathering Patterns of Ignitable Liquids with the Advanced Distillation Curve Method

Bruno

Allen

2013

J. RES. NATL. INST. STAN.

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One can take advantage of the striking similarity of ignitable liquid vaporization (or weathering) patterns and the separation observed during distillation to predict the composition of residual compounds in fire debris. This is done with the advanced distillation curve (ADC) metrology, which separates a complex fluid by distillation into fractions that are sampled, and for which thermodynamically consistent temperatures are measured at atmospheric pressure. The collected sample fractions can be analyzed by any method that is appropriate. Analytical methods we have applied include gas chromatography (with flame ionization, mass spectrometric and sulfur chemiluminescence detection), thin layer chromatography, FTIR, Karl Fischer coulombic titrimetry, refractometry, corrosivity analysis, neutron activation analysis and cold neutron prompt gamma activation analysis. We have applied this method on product streams such as finished fuels (gasoline, diesel fuels, aviation fuels, rocket propellants), crude oils (including a crude oil made from swine manure) and waste oils streams (used automotive and transformer oils). In this paper, we present results on a variety of ignitable liquids that are not commodity fuels, chosen from the Ignitable Liquids Reference Collection (ILRC). These measurements are assembled into a preliminary database. From this selection, we discuss the significance and forensic application of the temperature data grid and the composition explicit data channel of the ADC.

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Section: Ignitable Liquidsmentioning

confidence: 99%

Weathering Patterns of Ignitable Liquids with the Advanced Distillation Curve Method

Bruno

Allen

2013

J. RES. NATL. INST. STAN.

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“…Moreover, a particularly attractive feature of PLOT-cryo is the ability to simultaneously sample headspace with multiple, different sorbent phases (selected for their specific functionalities), including the clay and organoclay phases developed that are especially suited for aromatic compounds. 56 In the past, as many as eight separate phases have been used, simultaneously, to collect vapor from a single sample. Alternatively, the approach allows for sampling with multiple PLOT capillaries of the same phase, for repeatability and quality assurance.…”

Section: ■ Introductionmentioning

confidence: 99%

“…The PLOT capillaries are robust and inexpensive, and unlike other headspace collection methods, PLOT-cryo is especially applicable for relatively involatile solutes because it has a large temperature operability range. Moreover, a particularly attractive feature of PLOT-cryo is the ability to simultaneously sample headspace with multiple, different sorbent phases (selected for their specific functionalities), including the clay and organoclay phases developed that are especially suited for aromatic compounds . In the past, as many as eight separate phases have been used, simultaneously, to collect vapor from a single sample.…”

Section: Introductionmentioning

confidence: 99%

Composition of the C₆+ Fraction of Natural Gas by Multiple Porous Layer Open Tubular Capillaries Maintained at Low Temperatures

2016

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As the sources of natural gas become more diverse, the trace constituents of the C6+ fraction are of increasing interest. Analysis of fuel gas (including natural gas) for compounds with more than 6 carbon atoms (the C6+ fraction) has historically been complex and expensive. Hence, this is a procedure that is used most often in troubleshooting rather than for day-to-day operations. The C6+ fraction affects gas quality issues and safety considerations such as anomalies associated with odorization. Recent advances in dynamic headspace vapor collection can be applied to this analysis and provide a faster, less complex alternative for compositional determination of the C6+ fraction of natural gas. Porous layer open tubular capillaries maintained at low temperatures (PLOT-cryo) form the basis of a dynamic headspace sampling method that was developed at NIST initially for explosives in 2009. This method has been recently advanced by the combining of multiple PLOT capillary traps into one “bundle,” or wafer, resulting in a device that allows the rapid trapping of relatively large amounts of analyte. In this study, natural gas analytes were collected by flowing natural gas from the laboratory (gas out of the wall) or a prepared surrogate gas flowing through a chilled wafer. The analytes were then removed from the PLOT-cryo wafer by thermal desorption and subsequent flushing of the wafer with helium. Gas chromatography (GC) with mass spectrometry (MS) was then used to identify the analytes.

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“…This has included the clay and organoclay phases developed at NIST that are especially applicable for aromatic and sulfur compounds. [21][22][23][24] We have in fact used up to eight separate phases, simultaneously, to collect vapor from the headspace of a single sample. Alternatively, the approach allows sampling multiple samples with multiple PLOT capillaries of the same phase, for repeatability and quality assurance.…”

Section: Introductionmentioning

confidence: 99%

Field portable low temperature porous layer open tubular cryoadsorption headspace sampling and analysis part I: Instrumentation

Bruno

2016

Journal of Chromatography A

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Building on the successful application in the laboratory of PLOT-cryoadsorption as a means of collecting vapor (or headspace) samples for chromatographic analysis, in this paper a field portable apparatus is introduced. This device fits inside of a briefcase (aluminum tool carrier), and can be easily transported by vehicle or by air. The portable apparatus functions entirely on compressed air, making it suitable for use in locations lacking electrical power, and for use in flammable and explosive environments. The apparatus consists of four aspects: a field capable PLOT-capillary platform, the supporting equipment platform, the service interface between the PLOT-capillary and the supporting equipment, and the necessary peripherals. Vapor sampling can be done with either a hand piece (containing the PLOT capillary) or with a custom fabricated standoff module. Both the hand piece and the standoff module can be heated and cooled to facilitate vapor collection and subsequent vapor sample removal. The service interface between the support platform and the sampling units makes use of a unique counter current approach that minimizes loss of cooling and heating due to heat transfer with the surroundings (recuperative thermostatting). Several types of PLOT-capillary elements and sampling probes are described in this report. Applications to a variety of samples relevant to forensic and environmental analysis are discussed in a companion paper.

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Wall-coated open-tubular column chromatography on an organo–clay stationary phase

Cited by 15 publications

References 16 publications

Weathering Patterns of Ignitable Liquids with the Advanced Distillation Curve Method

Weathering Patterns of Ignitable Liquids with the Advanced Distillation Curve Method

Composition of the C₆+ Fraction of Natural Gas by Multiple Porous Layer Open Tubular Capillaries Maintained at Low Temperatures

Field portable low temperature porous layer open tubular cryoadsorption headspace sampling and analysis part I: Instrumentation

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Wall-coated open-tubular column chromatography on an organo–clay stationary phase

Cited by 15 publications

References 16 publications

Weathering Patterns of Ignitable Liquids with the Advanced Distillation Curve Method

Weathering Patterns of Ignitable Liquids with the Advanced Distillation Curve Method

Composition of the C6+ Fraction of Natural Gas by Multiple Porous Layer Open Tubular Capillaries Maintained at Low Temperatures

Field portable low temperature porous layer open tubular cryoadsorption headspace sampling and analysis part I: Instrumentation

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Product

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Composition of the C₆+ Fraction of Natural Gas by Multiple Porous Layer Open Tubular Capillaries Maintained at Low Temperatures