溶剂型木器涂料中卤代烃和乙二醇醚及醚酯类化合物含量的测定

Determination of Halogenated Hydrocarbons,Glycol Ethers and Ether Esters in Solvent-Based Wood Coatings

建立了气相色谱-质谱法测定溶剂型木器涂料中11种卤代烃和8种乙二醇醚及醚酯类化合物含量的方法。在1 g样品中加入10 mL甲醇,涡旋震荡混匀,于30℃水浴中超声提取30 min,离心分层,取上清液过0.45μm有机相滤膜;在离子源温度为230℃,选择离子监测(SIM)模式下进行测定,外标法定量。结果显示,在线性范围1.0~50 mg/L的范围内具有良好的线性关系,相关系数均>0.999。目标物的检出限(3S/N)在0.03~0.70μg/mL之间;对实际样品进行3个浓度水平的加标回收率试验,得到回收率在96.5%~103.5%之间,测定的相对标准偏差(n=7)在0.9%~5.6%之间。

A method for the determination of 11 halogenated hydrocarbons and 8 glycol ethers and ether esters in solvent-based wood coatings by gas chromatography-mass spectrometry is established.10mL methanol is added into 1g sample and is mixed evenly with vortex vibration,followed by ultrasonic extraction in 30℃water bath for 30 min,centrifugal stratification and filter through 0.45μm membrane.The ion source temperature is 230℃.The ion monitoring(SIM)mode is selected for determination,and the external standard method is used for quantification.It is revealed that there is a good linear relationship in the linear range of 1.0~50 mg/L,and the correlation coefficients are greater than 0.999.The detection limit(3S/N)of the target is 0.03-0.70μg/mL.The recoveries of the actual samples are tested at three concentration levels,and the recoveries are 96.5%-103.5%,and RSDs(n=7)of the determined values are ranged from 0.9%to 5.6%.