Increasing flame ionization detector (FID) sensitivity using post-column oxidation–methanation

Spanjers, Charles S.; Beach, Connor A.; Jones, Andrew; Dauenhauer, Paul J.

doi:10.1039/c6ay03363f

Cited by 34 publications

(22 citation statements)

References 20 publications

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“…Therefore, by applying Eq. , the carbon content and concentration can be easily determined without calibration and known response factors, simply by incorporating an internal standard (std) (IS) :

RF = 1 = \frac{mol C / area}{mol {normalC}_{std} / are {normala}_{std}} \Rightarrow mol normalC .

…”

Section: Introductionmentioning

confidence: 99%

Complex mixture quantification without calibration using gas chromatography and a comprehensive carbon reactor in conjunction with flame ionization detection

Bai

Carlton

Schug

2018

J of Separation Science

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Quantification of complex carbon-containing mixtures is typically a very time-intensive task with regards to the calibration process. A gas chromatograph with a flame ionization detector yields strong responses to organic compounds and provides a wide linear range over many orders of magnitude; however, responses for highly functionalized and heteroatom-containing compounds can be variable. Here, a commercial Polyarc microreactor unit, placed before the flame ionization detector, was investigated as a means of normalizing carbon response across all compounds. The device includes two catalytic reaction chambers, ultimately converting all carbon atoms to methane evenly for flame ionization detection. Three groups of different complex mixtures from n-alkane to terpene and polymer mixtures were analyzed to evaluate the potential for calibration-free quantitation of the new detector arrangement. We have obtained accurate quantification results without time-consuming calibration processes. The quantification of a terpene mixture and a polymer mixture confirms the ability of the detector for analyzing samples that either have complex physical or structural properties or wide concentration range. In summary, compared to other detectors, this methanizer - flame ionization detection system provides a simplified workflow, which can eliminate calibration steps and increase throughput.

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RF = 1 = \frac{mol C / area}{mol {normalC}_{std} / are {normala}_{std}} \Rightarrow mol normalC .

…”

Section: Introductionmentioning

confidence: 99%

Complex mixture quantification without calibration using gas chromatography and a comprehensive carbon reactor in conjunction with flame ionization detection

Bai

Carlton

Schug

2018

J of Separation Science

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“…[11][12][13][14] Applications of postcolumn reaction GC-FID systems have also been reported by other research groups. [15][16][17][18][19] In this system, target components separated by column are completely converted to carbon dioxide at the oxidizing part and then completely reduced to methane, followed by detection using the FID. Therefore, the sensitivity is proportional to the number of carbon atoms of a target component, irrespective of the compound, and it is not necessary to prepare all the standard materials related to the target components to calibrate the system.…”

Section: Introductionmentioning

confidence: 99%

“…13,14 Applications for measuring NOCs have been reported before. [17][18][19] However, performances of the determined values were not sufficient in accuracy and precision. The reported result had a too large error (over 8% relative) 17 compared with the hydrocarbons measurement results (relative standard uncertainties of measured values: 0.15 -2.10%), 15 and the obtained value was not proportional to the number of carbon atoms in the target component (the effective carbon number was 0.96 ± 0.01, not 1.00), 18 therefore it is presumed that there was some bias or fault in the results.…”

Section: Introductionmentioning

confidence: 99%

“…[17][18][19] However, performances of the determined values were not sufficient in accuracy and precision. The reported result had a too large error (over 8% relative) 17 compared with the hydrocarbons measurement results (relative standard uncertainties of measured values: 0.15 -2.10%), 15 and the obtained value was not proportional to the number of carbon atoms in the target component (the effective carbon number was 0.96 ± 0.01, not 1.00), 18 therefore it is presumed that there was some bias or fault in the results. Only the average measurement error (2.6%) and the estimated standard deviation of measurement error (0.91%) were shown, and concrete measurement errors of each target species were not indicated.…”

Section: Introductionmentioning

confidence: 99%

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Application and Validation of a Determination Method Using Post-column Reaction Gas Chromatography of Nitrogen-containing Organic Compounds

et al. 2018

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In this work, we applied post-column reaction gas chromatography (GC) using a flame ionization detector (FID) system to study nitrogen-containing organic compounds (NOCs). The results were subsequently validated. After separation by column, the target components were converted to carbon dioxide using an oxidizing catalyst and then reduced to methane, followed by detection using an FID. SI-traceable testing mixtures containing NOCs (isoprocarb, napropamide, and pendimethalin) were prepared by the gravimetric blending method. These mixtures were analyzed using a post-column reaction GC-FID system; standard materials of hydrocarbons were used as calibrants in this analysis. The determined values were compared with the values obtained for samples prepared at the corresponding concentrations, and statistical analyses were performed in all cases. It was shown that the determined and prepared values agreed well with each other within the uncertainty limits.

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“…Of special interest are organic mixtures rich in heteroatoms, including oxygen, sulfur, and nitrogen, which are more difficult to separate and detect by conventional gas chromatography techniques . Conventional detection of eluting compounds by flame ionization detection (FID) is significantly limited in quantifying chemicals with heteroatoms; for example, some oxygenates such as formaldehyde or formic acid are almost undetectable . Advanced gas chromatography methods that address both limitations and enable rapid quantitative analysis of complex mixtures containing a large number of organic compounds are in high demand for applications in biofuels, clean water, and new consumer products …”

Section: Introductionmentioning

confidence: 99%

Complete carbon analysis of sulfur‐containing mixtures using postcolumn reaction and flame ionization detection

et al. 2017

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Quantitative analysis of complex mixtures containing hundreds-to-thousands of organic compounds rich in heteroatoms, including oxygen, sulfur, and nitrogen, is a major challenge in the fuel, food, and chemical industries. In this work, a two-stage (oxidation and methanation) catalytic process in a 3-D-printed metal microreactor was evaluated for its capability to convert sulfur-containing organic compounds to methane. The microreactor was inserted into a gas chromatograph between the capillary column and flame ionization detector. Catalytic conversion of all sulfur-containing analytes to methane enabled carbon quantification without calibration, by the method identified as "quantitative carbon detection" or QCD. Quantification of tetrahydrothiophene, dimethyl sulfoxide, diethyl sulfide, and thiophene indicated complete conversion to methane at 4508C. Long-term performance of a commercial microreactor was evaluated for 2000 consecutive injections of sulfur-containing organic analytes. The sulfur processing capacity of the microreactor was identified experimentally, after which reduced conversion to methane was observed.

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Increasing flame ionization detector (FID) sensitivity using post-column oxidation–methanation

Abstract: Combining a microreactor with the flame ionization detector (FID) greatly increases its response to highly oxidized organic molecules.

Cited by 34 publications

References 20 publications

Complex mixture quantification without calibration using gas chromatography and a comprehensive carbon reactor in conjunction with flame ionization detection

Complex mixture quantification without calibration using gas chromatography and a comprehensive carbon reactor in conjunction with flame ionization detection

Application and Validation of a Determination Method Using Post-column Reaction Gas Chromatography of Nitrogen-containing Organic Compounds

Complete carbon analysis of sulfur‐containing mixtures using postcolumn reaction and flame ionization detection

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