Procedure for testing inertness of inserts and insert packing materials for GC injectors

Grob, Konrad; Wagner, Christoph

doi:10.1002/jhrc.1240160804

Cited by 15 publications

(6 citation statements)

References 9 publications

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“…These compounds are also the least abundant in the matrix with concentrations of only 117 and 184 ng g -1 . The recoveries of the PAH are, however, comparable with those in other studies [17,18], and the results are reasonable for environmental analysis.…”

Section: Pahsupporting

confidence: 84%

“…DDT is a thermolabile compound that can be degraded during gas chromatographic analysis [17,18]. For example, the analysis of 4,4'-DDT-d 8 , the surrogate standard used for the quantification of chlorinated pesticides under the conditions used for the analysis of PCB leads to the detection of three peaks (Fig.…”

Section: Optimisation Of Gas Chromatographic Injector Conditions For mentioning

confidence: 99%

“…Similarly, the analysis of DDT by gas chromatographic methods can be a challenging task [17,18]. DDT is a relatively thermolabile compound and the high injector temperatures used in gas chromatography can cause degradation during the analysis.…”

Section: Introductionmentioning

confidence: 99%

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Multi-residue analysis of polycyclic aromatic hydrocarbons, polychlorobiphenyls, and organochlorine pesticides in marine sediments

et al. 2001

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A multi-residue analysis procedure using microwave-assisted extraction and pre-purification has been developed for the combined analysis of polycyclic aromatic hydrocarbons (PAH), polychlorobiphenyls (PCB), and organochlorine pesticides (OCP) in marine sediments. This procedure has been validated with certified marine sediment. Several surrogate standards have been employed and the use of octachloronaphthalene (OCN) as a surrogate standard for organochlorine determination in this matrix is discussed. The recoveries of all compounds were high (>70%) and the relative standard deviations are of the same order as the certified values. Different analytical problems are discussed, including DDT degradation in gas chromatography and laboratory PCB background levels. Quantification problems encountered for two pesticides (cis-chlordane and trans-nonachlor) were attributed to PAH interference in the GC-ECD chromatogram.

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Section: Pahsupporting

confidence: 84%

Section: Optimisation Of Gas Chromatographic Injector Conditions For mentioning

confidence: 99%

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Multi-residue analysis of polycyclic aromatic hydrocarbons, polychlorobiphenyls, and organochlorine pesticides in marine sediments

et al. 2001

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“…The laminar liner shows better chromatographic performance [21], but does not reliably arrest 20 -50 lL of sample liquid. This dilemma is not new: deactivated glass or fused silica wool performs perfectly for the injection of non-adsorptive, stable compounds, but insufficient inertness has been described for conventional splitless injection [23] as well as for programmed temperature vaporizing injection (PTV) [24,25].…”

Section: Discussionmentioning

confidence: 99%

Large volume splitless injection with concurrent solvent recondensation: Keeping the sample in place in the hot vaporizing chamber

Biedermann¹,

Fiscalini²,

Grob³

2004

J of Separation Science

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An injector liner packed with a plug of glass wool is compared with a laminar and a mini laminar liner for large volume (20-50 microL) splitless injection with concurrent solvent recondensation (CSR-LV splitless injection). Videos from experiments with perylene solutions injected into imitation injectors show that glass wool perfectly arrested the sample liquid and kept it in place until the solvent had evaporated. The sample must be transferred from the needle to the glass wool as a band, avoiding 'thermospraying' by partial solvent evaporation inside the needle. The liquid contacted the liner wall when the band was directed towards it, but from there it was largely diverted to the glass wool. In the laminar liners, part of the liquid remained and evaporated at the entrance of the obstacle, while the other proceeded to the center cavity. Vapors formed in the center cavity drove liquid from the entrance of the obstacle upwards, but the importance of such problems could not be verified in the real injector. Some liquid split into small droplets broke through the obstacle and entered the column. Breakthrough through the laminar liners was confirmed by a chromatographic experiment. An improved design of a laminar liner for large volume injection is discussed as a promising alternative if glass wool causes problems originating from insufficient inertness.

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“…Figure 2 shows the peak areas obtained after injection of 0.5 ng of each pesticide by conventional splitless (2 gL) and by PTV injection (50 pL) with and without glass-wool packing. Some authors report that glass wool is not suitable as a packing material because even silanized wool is not sufficiently inert and causes thermal degradation o f labile analytes and adsorption o f polar analytes [24] (Tenax is usually preferred [5,9,17].) Some authors report that glass wool is not suitable as a packing material because even silanized wool is not sufficiently inert and causes thermal degradation o f labile analytes and adsorption o f polar analytes [24] (Tenax is usually preferred [5,9,17].)…”

Section: Optimization Of Ptv Inj Ectionmentioning

confidence: 99%

Multiresidue procedures for determination of triazine and organophosphorus pesticides in water by use of large-volume PTV injection in gas chromatography

et al. 2000

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Two procedures, based on large-volume injection with a programmed-temperature vaporizer (PTV), have been developed for the determination of several triazine and organophosphorus pesticides. The use of PTV for injection in gas chromatography (GC) has enabled the introduction of up to 200 ~L sample extract into the GC, thus increasing the sensitivity of the method. PTV injection has been combined off-line with two different microextraction procedures liquid-liquid partition and solid-phase extraction. A simple and rapid off-line liquid-liquid microextraction procedure (5 mL water/1 mL methyl tert-butyl ether) was applied to surface water samples spiked at levels between 0.01 and 5 #gL -1. Recoveries of the overall procedure were >80% and the precision was better than 15 %. Detection limits were <30 ng L 1 from 200-#L injections in GC-NPD analysis of triazines and GC-FPD analysis of organophosphorus pesticides. Off-line automated solidphase extraction with Cls cartridges has been applied to water samples (50 mL) spiked at 0.01, 0.1 and 1 #g L 1. The overall procedure was satisfactory (recoveries >80 % and coefficients of variation <12 %) and the limits of detection ranged from 1 to 9 ng L 1. Finally, several surface water samples were analysed, and triazine herbicides were detected at concentrations of approx. 0.1 0.2 #g L 1. The results were similar to those obtained by conventional solvent extraction then GC-MSD after splitless injection of 2/~L.

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Procedure for testing inertness of inserts and insert packing materials for GC injectors

Cited by 15 publications

References 9 publications

Multi-residue analysis of polycyclic aromatic hydrocarbons, polychlorobiphenyls, and organochlorine pesticides in marine sediments

Multi-residue analysis of polycyclic aromatic hydrocarbons, polychlorobiphenyls, and organochlorine pesticides in marine sediments

Large volume splitless injection with concurrent solvent recondensation: Keeping the sample in place in the hot vaporizing chamber

Multiresidue procedures for determination of triazine and organophosphorus pesticides in water by use of large-volume PTV injection in gas chromatography

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