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Precise and Accurate Compound Specific Carbon andNitrogen Isotope Analysis of Atrazine: Critical Role of CombustionOven Conditions
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n2:meyerarminh n9:person n2:penningholger n2:lowagharald
dcterms:abstract
A Ni/NiO combustion interface accomplishes accurate andprecise carbon and nitrogen isotope analysis of atrazine by gas chromatography-isotoperatio mass spectrometry and allows determination of isotope fractionationduring alkaline hydrolysis. Compound-specific stable isotope analysis by gas chromatography-isotoperatio mass spectrometry (GC-IRMS) is increasingly used to assess originand fate of organic substances in the environment. Although analysiswithout isotopic discrimination is essential, it cannot be taken forgranted for new target compounds. We developed and validated carbonisotope analysis of atrazine, a herbicide widely used in agriculture.Combustion was tested with reactors containing (i) CuO/NiO/Pt operatingat 940 °C; (ii) CuO operating at 800 °C; (iii) Ni/NiO operatingat 1150 °C and being reoxidized for 2 min during each gas chromatographicrun. Accurate and precise carbon isotope measurements were only obtainedwith Ni/NiO reactors giving a mean deviation Δδ13C from dual inlet measurements of −0.1−0.2‰and a standard deviation (SD) of ±0.4‰. CuO at 800 °Cgave precise, but inaccurate values (Δδ13C= −1.3‰, SD ±0.4‰), whereas CuO/NiO/Pt reactorsat 940 °C gave inaccurate and imprecise data. Accurate (Δδ15N = 0.2‰) and precise (SD ±0.3‰)nitrogen isotope analysis was accomplished with a Ni/NiO-reactor previouslyused for carbon isotope analysis. The applicability of the methodwas demonstrated for alkaline hydrolysis of atrazine at 20 °Cand pH 12 (nucleophilic aromatic substitution) giving ϵcarbon = −5.6‰ ± 0.1‰ (SD) and ϵnitrogen = −1.2‰ ± 0.1‰ (SD).
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