Comparison of total vaporisation and dynamic headspace techniques combined with direct mass spectrometric detection for the on-line analysis of liquid process streams

Dunn, Warwick B.; Townshend, Alan; Green, John D.

doi:10.1039/a705516a

Cited by 7 publications

(4 citation statements)

References 18 publications

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“…Applications of headspace analysis benefit either from the simplicity of automation or from removing some of the matrix effects. However, one study found that even dynamic headspace techniques could not eliminate the effect of the sample matrix on analysis if the analytes were incompletely extracted [63]. A table comparing the advantages and disadvantages of these techniques is available in our previous study [51].…”

Section: Sample Extractionmentioning

confidence: 99%

Application of Comprehensive 2D Gas Chromatography Coupled with Mass Spectrometry in Beer and Wine VOC Analysis

et al. 2023

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To meet consumer demand for fermented beverages with a wide range of flavors, as well as for quality assurance, it is important to characterize volatiles and their relationships with raw materials, microbial and fermentation processes, and the aging process. Sample preparation techniques coupled with comprehensive 2D gas chromatography (GC×GC) and mass spectrometry (MS) are proven techniques for the identification and quantification of various volatiles in fermented beverages. A few articles discuss the application of GC×GC for the measurement of fermented beverage volatiles and the problems faced in the experimental analysis. This review critically discusses each step of GC×GC-MS workflow in the specific context of fermented beverage volatiles’ research, including the most frequently applied volatile extraction techniques, GC×GC instrument setup, and data handling. The application of novel sampling techniques to shorten preparation times and increase analytical sensitivity is discussed. The pros and cons of thermal and flow modulators are evaluated, and emphasis is given to the use of polar-semipolar configurations to enhance detection limits. The most relevant Design of Experiment (DoE) strategies for GC×GC parameter optimization as well as data processing procedures are reported and discussed. Finally, some consideration of the current state of the art and future perspective, including the crucial role of AI and chemometrics.

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Section: Sample Extractionmentioning

confidence: 99%

Application of Comprehensive 2D Gas Chromatography Coupled with Mass Spectrometry in Beer and Wine VOC Analysis

et al. 2023

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“…The matrix effect influences the volatility of each dissolved compound to a different degree; therefore, the purge time needed to achieve an exhaustive extraction for each compound will also vary. Dunn et al [33] have found that the dynamic headspace technique suffers from dependence of the calibration data on the sample matrix composition, thus making complicated multivariate calibration techniques necessary to obtain accurate results.…”

Section: Comparison Of Static Hs-gc With Pandtmentioning

confidence: 99%

General Introduction

2006

Static Headspace–Gas Chromatography

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“…Thermal vaporisation of discrete liquid samples into a process mass spectrometer has been achieved using heated auto-injection valves [34][35][36], a modified GC oven [37], and a programmable temperature vaporizing (PTV) GC injector and syringe pump [38]. However, these methods are not ideal for continuous sampling; when a carrier gas is used to transport the sample vapours to the mass spectrometer variations in the carrier gas flow and inefficient mixing with the sample vapour can cause signal instability.…”

Section: Introductionmentioning

confidence: 99%

Monitoring of an esterification reaction by on-line direct liquid sampling mass spectrometry and in-line mid infrared spectrometry with an attenuated total reflectance probe

Owen

McAulay

Nordon

et al. 2014

Analytica Chimica Acta

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A specially designed thermal vaporiser was used with a process mass spectrometer designed for gas analysis to monitor the esterification of butan-1-ol and acetic anhydride. The reaction was conducted at two scales: in a 150 mL flask and a 1L jacketed batch reactor, with liquid delivery flow rates to the vaporiser of 0.1 and 1.0 mLmin(-1), respectively. Mass spectrometry measurements were made at selected ion masses, and classical least squares multivariate linear regression was used to produce concentration profiles for the reactants, products and catalyst. The extent of reaction was obtained from the butyl acetate profile and found to be 83% and 76% at 40°C and 20°C, respectively, at the 1L scale. Reactions in the 1L reactor were also monitored by in-line mid-infrared (MIR) spectrometry; off-line gas chromatography (GC) was used as a reference technique when building partial least squares (PLS) multivariate calibration models for prediction of butyl acetate concentrations from the MIR spectra. In validation experiments, good agreement was achieved between the concentration of butyl acetate obtained from in-line MIR spectra and off-line GC. In the initial few minutes of the reaction the profiles for butyl acetate derived from on-line direct liquid sampling mass spectrometry (DLSMS) differed from those of in-line MIR spectrometry owing to the 2 min transfer time between the reactor and mass spectrometer. As the reaction proceeded, however, the difference between the concentration profiles became less noticeable. DLSMS had advantages over in-line MIR spectrometry as it was easier to generate concentration profiles for all the components in the reaction. Also, it was possible to detect the presence of a simulated impurity of ethanol (at levels of 2.6 and 9.1% mol/mol) in butan-1-ol, and the resulting production of ethyl acetate, by DLSMS, but not by in-line MIR spectrometry.

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Comparison of total vaporisation and dynamic headspace techniques combined with direct mass spectrometric detection for the on-line analysis of liquid process streams

Cited by 7 publications

References 18 publications

Application of Comprehensive 2D Gas Chromatography Coupled with Mass Spectrometry in Beer and Wine VOC Analysis

Application of Comprehensive 2D Gas Chromatography Coupled with Mass Spectrometry in Beer and Wine VOC Analysis

General Introduction

Monitoring of an esterification reaction by on-line direct liquid sampling mass spectrometry and in-line mid infrared spectrometry with an attenuated total reflectance probe

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