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Development and Validation of Novel DH-GC-ITMS Methods for the Determination of Freon F-141b in Formulated Polyol and Rigid Polyurethane Foam

机译:DH-GC-ITMS新方法的开发与验证,用于测定配制的多元醇和硬质聚氨酯泡沫中的氟利昂F-141b

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摘要

Two efficient methods for the determination of 1,1-dichloro-1-fluoroethane (Freon F-141b) in formulated polyol and rigid polyurethane foam by dynamic-headspace-gas chromatography-ion trap-mass spectrometry were developed and validated. Rigid polyurethane foam was efficiently dissolved in dimethylformamide by heating at the temperature of 60 °C for 2 h.Validation was carried out in terms of limits of detection (LOD), limits of quantitation (LOQ), linearity, precision and recovery. LOD values of 4.00 μg kg−1 for rigid polyurethane foam and 0.73 μg kg−1 for formulated polyol were achieved, whereas linearity was statistically verified over one order of magnitude. Precision was evaluated testing two concentration levels. Good results were obtained both in terms of intra-day repeatability and between-day precision: RSD % lower than 4% (n = 6) at the concentration of 15 μg kg−1 were calculated for intra-day repeatability. Extraction recoveries up to 92.6±1.6 % (n = 3) were also calculated by the addition of Freon F-141b to the samples analysed. Both the methods were applied for the analysis of a number of formulated polyol and rigid polyurethane foam samples.
机译:建立并验证了动态顶空-气相色谱-离子阱质谱法测定配制的多元醇和硬质聚氨酯泡沫塑料中1,1-二氯-1-氟乙烷(Freon F-141b)的两种有效方法。通过在60°C的温度下加热2小时将硬质聚氨酯泡沫有效地溶解在二甲基甲酰胺中。根据检测限(LOD),定量限(LOQ),线性,精密度和回收率进行验证。硬质聚氨酯泡沫的LOD值为4.00μgkg-1 ,配制的多元醇的LOD值为0.73μgkg-1 ,而线性度在一个数量级上得到了统计验证。通过测试两个浓度水平来评估精度。在日内重复性和日间精度方面均取得了良好的结果:计算出日内重复性在15μgkg-1

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