State Key Laboratory of Pulp and Paper Engineering, South China University of Technology, Guangzhou, Guangdong 510640, China.
J Chromatogr A. 2012 Jan 27;1222:1-4. doi: 10.1016/j.chroma.2011.11.045. Epub 2011 Dec 19.
This paper reports on a desiccated full evaporation headspace gas chromatographic (FE HS-GC) technique for determination of the methanol content in dilute mill effluents. Anhydrous K(2)CO(3) was selected as the preferred salt for eliminating the water in the sample in the headspace sample vial. The results showed that the addition of 12 g K(2)CO(3) made it possible to introduce a larger sample size (up to 1 mL) into the FE HS-GC measurement, thereby increasing the sensitivity of the technique. At the given equilibration temperature (105°C), a near-complete mass transfer of methanol from the liquid phase to vapor phase (headspace) was achieved within 10 min. Replicate samples showed that the relative standard deviation of the method was less than 1.5%. Further, the limit of quantification (LOQ) was 0.12 μg and the recovery ranged from 95 to 104%. The present method greatly improves the methanol detection sensitivity in the FE HS-GC method and has the added advantage of being simple, rapid and accurate.
本文报道了一种用于测定稀浆流中甲醇含量的干燥全蒸发顶空气相色谱（FE HS-GC）技术。无水 K(2)CO(3)被选为顶空样品瓶中用于去除样品中水分的首选盐。结果表明，加入 12 g K(2)CO(3)使得可以将更大的样品量（高达 1 mL）引入 FE HS-GC 测量中，从而提高了该技术的灵敏度。在给定的平衡温度（105°C）下，甲醇从液相到气相（顶空）的近乎完全传质在 10 分钟内完成。重复样品表明，该方法的相对标准偏差小于 1.5%。此外，定量限（LOQ）为 0.12 μg，回收率范围为 95%至 104%。本方法极大地提高了 FE HS-GC 方法中甲醇检测的灵敏度，并且具有简单、快速和准确的优点。
