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    Vergelijking bepaling minerale olie in sediment met gaschromatografie en infraroodspectrometrie

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    Authors
    de Jong APJM
    van der Heeft E
    Visser T
    Type
    Report
    Language
    nl
    
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    Title
    Vergelijking bepaling minerale olie in sediment met gaschromatografie en infraroodspectrometrie
    Translated Title
    Comparison on the analysis of mineral oil in sediment by gas chromatography and infrared spectrometry
    Publiekssamenvatting
    Vergelijkend onderzoek is verricht naar de bepaling van minerale olien in sediment en water met behulp van infraroodspectrometrie (IR) en gaschromatografie (GC) conform de NEN-voorschriften 5733 en 6675. Daarnaast zijn modificaties ter verbetering van deze methoden bestudeerd. In een toepassing op sedimentmonsters met een gehalte van circa 0.5-1 g/kg ds, gaf de GC-bepaling gemiddeld een 20 % hoger resultaat (range 6-32%) dan IR. Oorzaken hiervoor zijn niet gevonden. Veranderingen van de bestaande NEN voorschriften zijn uitgevoerd met betrekking tot (1) verwijdering van dissolved organic carbon (DOC) macromoleculaire co-extractanten ; (2) gebruik van pentaan ter vervanging van gehalogeneerde koowaterstoffen als extractiemiddel ; (3) verwijdering van laag tot medium moleculaire polaire stoffen uit extracten door middel van terug-extractie in een verdunde loogoplossing. Geen van de modificaties resulteerde in een significant ander resultaat dan behaald met de normmethode. Op grond hiervan wordt geconcludeerd dat: (1) de huidige voorschriften voorzien in een betrouwbare analyse van minerale olie in sediment en water ; (2) de IR en de GC methode tot goed vergelijkbare resultaten leiden vanaf gehalten >0.2-0.5 mg/kg ; (3) verbetering van de methoden gericht op verlaging van het risico op vals positieve resultaten niet met eenvoudige middelen kan worden bereikt ; (4) pentaan als alternatief extractiemiddel kan worden gebruikt na een eventueel verbod op het gebruik van Freon-113 en ander gehalogeneerde koolwaterstoffen.<br>
    A comparitive study has been carried out on the analysis of mineral oil in sediment and water samples by gas chromatography (GC) and infrared spectrometry (IR) according to the current standard methods NEN 5733 and 6675. In an application to sediment samples, results obtained with GC analysis were found to be about 20% higher compared to the IR method (range +6 to +32%). Causes for these differences were not found. Additionally, modifications to improve the performance of the NEN-procedures were investigated. Changes comprised (1) repeated removal of co-extracted dissolved organic carbon (DOC) ; (2) the use of pentaine instead of Freon-113 as extraction solvent and (3) alkaline aqueous washing (back-extraction) of extracts to remove small to medium size acidic co-extractants. However, results obtained were not essentially different from those obtained with the standard method. Based on that, the following conclusions were drawn: (1) the present standard procedures can be considered as reliable methods for the analysis of mineral oil in water en sediment samples, (2) the performance of the GC and IR method is comparable in applications above the determination limit of the latter (0.2-.5 mg/kg) ; (3) improvement of the current standards cannot be achieved with relative simple means; (4) pentane is an acceptable alternative for Freon-113 and other halogenated hydrocarbons in case these solvents are banned for analytical use.<br>
    Publisher
    Rijksinstituut voor Volksgezondheid en Milieu RIVM
    Sponsors
    HIMH
    URI
    http://hdl.handle.net/10029/255988
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