Determination of SCFAs in water using GC-FID. Selection of the separation system

Banel, Anna; Jakimska, A.; Wasielewska, Marta; Wolska, Lidia; Zygmunt, Bogdan

doi:10.1016/j.aca.2011.02.059

Cited by 18 publications

(6 citation statements)

References 16 publications

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“…These peaks are difficult to integrate reliably and often lead to reduced analyte response. 22,23 The peak shapes of polar compounds such as amines are particularly sensitive to active sites in gas chromatographs (such as exposed silica and deposits in inlet liners or columns) and dipole−dipole or ionic interactions with the column phase. 21,22 The widths and asymmetry factors of the MEA peak on five different column phases are reported in Table 2.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

“…Established GC methods for measuring the concentrations of acidic polar organic compounds in aqueous matrixes are widely available in the peer-reviewed literature, − but very little information is available for the analysis of basic compounds in aqueous matrixes. In this study, the most appropriate column phases were selected by comparing the MEA peak shapes on five different column phases.…”

Section: Resultsmentioning

confidence: 99%

“…Strongly tailing peaks indicate severe interactions between the analyte and the chromatographic system. These peaks are difficult to integrate reliably and often lead to reduced analyte response. , The peak shapes of polar compounds such as amines are particularly sensitive to active sites in gas chromatographs (such as exposed silica and deposits in inlet liners or columns) and dipole–dipole or ionic interactions with the column phase. , The widths and asymmetry factors of the MEA peak on five different column phases are reported in Table . The mass of MEA injected onto each column and the column oven temperature program were varied to provide each column with a fair chance of producing a MEA peak with a good peak shape.…”

Section: Resultsmentioning

confidence: 99%

“…Acidification of aqueous matrixes prior to the analysis of short-chain fatty acids is commonly used to prevent ionization and ensure reproducible recovery of the analytes. − In this study, all samples and standards were diluted 1:1000 in a volatile buffer (0.1% ammonium hydroxide) to convert MEA to its neutral form, ensure that the pH values of samples and standards were consistent, and shield MEA from acidic sites in the GC system. The increased MEA response in the presence of ammonium hydroxide is evident in Figure .…”

Section: Resultsmentioning

confidence: 99%

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Quantification of Aqueous Monoethanolamine Concentration by Gas Chromatography for Postcombustion Capture of CO₂

Reynolds

Verheyen

Adeloju

et al. 2014

Ind. Eng. Chem. Res.

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The availability of reliable analytical methods for measuring amine concentrations is necessary for optimum operation of aqueous amine CO2 separation systems being employed for postcombustion capture (PCC) of CO2. A GC-FID (gas chromatography with flame ionization detection) method is described for the reliable quantification of 30% (w/w) monoethanolamine (MEA) in severely degraded solvent samples. The observation of intermittent splitting of the MEA peak was a major concern with this approach. The use of a wide-bore column led to improved MEA peak resolution and peak shape. The reliability and robustness of the GC-FID method were assessed by analyzing degraded 30% (w/w) MEA solvent samples from CSIRO’s pilot plant at AGL’s Loy Yang power station in Victoria, Australia. The results were compared with those obtained by titration and total organic carbon (TOC) measurements of the same samples. The MEA concentrations obtained by the GC-FID and titration methods were statistically similar. In contrast, the MEA concentrations calculated from TOC were consistently higher than those obtained by both GC-FID and titration.

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Section: ■ Results and Discussionmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

See 2 more Smart Citations

Quantification of Aqueous Monoethanolamine Concentration by Gas Chromatography for Postcombustion Capture of CO₂

Reynolds

Verheyen

Adeloju

et al. 2014

Ind. Eng. Chem. Res.

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“…For this reason, the measurement of SCFA in biogas production has been recognized as a quantitative indicator for monitoring biogas production efficiency (Sheveleva andRamenskaya 2010, Madsen, Holm-Nielsen et al 2011). Thus, the monitoring of SCFAs produced by microbial samples is necessary for various reasons and it can be measured from a culture medium which is required for microbial growth (Banel, Jakimska et al 2012).…”

Section: Introductionmentioning

confidence: 99%

Method development for the quantitative determination of short chain fatty acids in microbial samples by solid phase extraction and gas chromatography with flame ionization detection

et al. 2019

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Background: In order to quantitatively measure short chain fatty acids (SCFAs) in microbial samples, sample preparation and analytical conditions using gas chromatography with flame ionization detection (GC-FID) were established. Methods: The extraction of SCFAs with ethyl ether-hexane (1:1, v/v) followed by the aminopropyl solid phase extraction (SPE) was carried out. An acid-modified poly(ethylene glycol) GC column was used for the chromatographic separation of four volatile fatty acids. Results: Good linearity was obtained with r > 0.999 in the calibration range. The limits of quantification (LOQs) of the analytical method were in the ranges of 5.71 to 11.20 μg/mL. The overall recoveries excluding acetic acid ranged between 96.51 and 108.83% with relative standard deviations (RSD) below 10% for the entire procedure from the results of matrix spiking experiments at three concentration levels. Conclusion: The analytical method was validated in accordance with the requirements of the international guideline. The method enables the use of the most commonly used technology without derivatization and the elimination of interferences in the sample matrix.

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An assessment of the liquid–gas partitioning behavior of major wastewater odorants using two comparative experimental approaches: liquid sample-based vaporization vs. impinger-based dynamic headspace extraction into sorbent tubes

et al. 2013

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The gas-liquid partitioning behavior of major odorants (acetic acid, propionic acid, isobutyric acid, n-butyric acid, i-valeric acid, n-valeric acid, hexanoic acid, phenol, p-cresol, indole, skatole, and toluene (as a reference)) commonly found in microbially digested wastewaters was investigated by two experimental approaches. Firstly, a simple vaporization method was applied to measure the target odorants dissolved in liquid samples with the aid of sorbent tube/thermal desorption/gas chromatography/mass spectrometry. As an alternative method, an impinger-based dynamic headspace sampling method was also explored to measure the partitioning of target odorants between the gas and liquid phases with the same detection system. The relative extraction efficiency (in percent) of the odorants by dynamic headspace sampling was estimated against the calibration results derived by the vaporization method. Finally, the concentrations of the major odorants in real digested wastewater samples were also analyzed using both analytical approaches. Through a parallel application of the two experimental methods, we intended to develop an experimental approach to be able to assess the liquid-to-gas phase partitioning behavior of major odorants in a complex wastewater system. The relative sensitivity of the two methods expressed in terms of response factor ratios (RFvap/RFimp) of liquid standard calibration between vaporization and impinger-based calibrations varied widely from 981 (skatole) to 6,022 (acetic acid). Comparison of this relative sensitivity thus highlights the rather low extraction efficiency of the highly soluble and more acidic odorants from wastewater samples in dynamic headspace sampling.

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Determination of SCFAs in water using GC-FID. Selection of the separation system

Cited by 18 publications

References 16 publications

Quantification of Aqueous Monoethanolamine Concentration by Gas Chromatography for Postcombustion Capture of CO₂

Quantification of Aqueous Monoethanolamine Concentration by Gas Chromatography for Postcombustion Capture of CO₂

Method development for the quantitative determination of short chain fatty acids in microbial samples by solid phase extraction and gas chromatography with flame ionization detection

An assessment of the liquid–gas partitioning behavior of major wastewater odorants using two comparative experimental approaches: liquid sample-based vaporization vs. impinger-based dynamic headspace extraction into sorbent tubes

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Determination of SCFAs in water using GC-FID. Selection of the separation system

Cited by 18 publications

References 16 publications

Quantification of Aqueous Monoethanolamine Concentration by Gas Chromatography for Postcombustion Capture of CO2

Quantification of Aqueous Monoethanolamine Concentration by Gas Chromatography for Postcombustion Capture of CO2

Method development for the quantitative determination of short chain fatty acids in microbial samples by solid phase extraction and gas chromatography with flame ionization detection

An assessment of the liquid–gas partitioning behavior of major wastewater odorants using two comparative experimental approaches: liquid sample-based vaporization vs. impinger-based dynamic headspace extraction into sorbent tubes

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Quantification of Aqueous Monoethanolamine Concentration by Gas Chromatography for Postcombustion Capture of CO₂

Quantification of Aqueous Monoethanolamine Concentration by Gas Chromatography for Postcombustion Capture of CO₂