１ 前 言
丙烯酸树脂残余单体的存在，使树脂气味大，导致自然环境受到污染，空气质量恶化，危害人们的健康，而且影响涂料涂膜的性能和应用。因而对丙烯酸残余单体进行分析，可以了解树脂的转化率，为工艺控制和配方调整提供依据，以便最大限度地降低残余单体的含量。目前，关于丙烯酸树脂残余单体含量的检测还没有国家标准和行业标准方法，而本方法采用气相谱法（氢火焰离子化检测器）使丙烯酸树脂中残余单体得到较好分离，灵敏度高，重现性好，能够定量检测残余单体含量，应用于丙烯酸树脂的科研与生产中，取得满意效果。 ２ 实验部分
２．１ 仪器
ＳＣ—１００１气相谱仪：配有氢火焰离子化检测器（ＦＩＤ）；
谱柱：５％ １，２—丙二醇己二酸聚酯填充柱，３ｍｍ×２ｍ；
微量注射器：１０μＬ，５０μＬ；
配样瓶：１０ｍＬ，具有可密封瓶塞；
移液管：５ｍＬ。
２．２ 试剂和材料
载气：氮气，纯度≥９９．８％；燃气：氢气，纯度≥９９．８％；助燃气：空气；乙酸丁酯，甲基丙烯酸甲酯（ＭＭＡ），丙烯酸丁酯（ＢＡ），苯乙烯（Ｓｔ），丙烯酸—β—羟丙酯（ＨＰＡ），丙烯酸（ＡＡ），均为分析纯。２．３ 样品前处理 ２．３．１ 稀释样品
精确称取样品１ ｇ左右（精确至０．０００２ｇ）于配样瓶中，再称取４ｇ左右乙酸丁酯，使样品
完全溶解在乙酸丁酯中，备用。
２．３．２ 标准样品的配制
用移液管取５ｍＬ乙酸丁酯于配样瓶中，再用微量注射器按表１所示的体积数将分析纯的甲基丙烯酸甲酯、丙烯酸丁酯、苯乙烯、丙烯酸—β—羟丙酯、丙烯酸加入到配样瓶中，精确称取所有化合物的总质
周亚莉（重庆三峡油漆股份有限公司，４０００５１）
摘要：乙酸丁酯稀释丙烯酸树脂后，用气相谱法使丙烯酸树脂中的各种残余单体得到较好分离，再
采用氢火焰离子化检测器（ＦＩＤ）定量测定。该方法灵敏度高，重现性好，应用于丙烯酸树脂的科研与生产中，取得满意效果。
关键词：气相谱法；残余单体；丙烯酸树脂；氢火焰离子化检测器（ＦＩＤ）
中图分类号：ＴＱ６３０．７＋２ 文献标识码：Ｂ 文章编号：１００６－２５５６（２００６）０３－００３３－０２
量为４．４１３ｇ，并充分摇匀（此标准样品当天配制）。２．４ 谱测定
２．４．１ 谱条件
载气（Ｎ２）流速：１５ｍＬ／ｍｉｎ；燃气（Ｈ２）流速：６０ ｍＬ／ｍｉｎ；助燃气（空气）流速：４００ ｍＬ／ｍｉｎ；汽化室温度：２００℃；检测器温度：２００℃；柱温：１２０℃（１５ｍｉｎ），１８０℃（２０ｍｉｎ）；升温速率：３０℃／ｍｉｎ。２．４．２ 测定
待仪器稳定后，吸取１μＬ标准样品注入汽化室，记录谱图和谱数据。
表１ 标样中各物质体积及浓度
HINA PAINT 2006.03
中国涂料
C
在同样条件下，吸取１μＬ稀释后的样品注入汽化室，记录谱图和谱数据。用外标法计算。
３ 结果与讨论
３．１ 谱分离
按上述条件操作，得到图３结果，丙烯酸树脂中各个残余单体（甲基丙烯酸甲酯、丙烯酸丁酯、苯乙烯、丙烯酸—β—羟丙酯、丙烯酸）的分离情况满足分析要求。
峰１—甲基丙烯酸甲酯（ＭＭＡ） 峰２—杂质峰峰３—乙酸丁酯 峰４—丙烯酸丁酯（ＢＡ）
峰５—苯乙烯（Ｓｔ） 峰６—丙烯酸—β—羟丙酯（ＨＰＡ）峰７—丙烯酸（ＡＡ）
图３ 丙烯酸树脂中各个残余单体的气相谱图
ＭＡ）、丙烯、苯乙烯（Ｓｔ）、丙烯酸—β—羟丙酯、丙烯酸（ＡＡ）的浓度（ｇ／ｋｇ）分别按下ｉ，丙烯酸树脂中ＭＭＡ、ＢＡ、Ｓｔ、ＨＰＡ、ｉ，样品中ＭＭＡ、ＢＡ、Ｓｔ、ＨＰＡ、ＡＡ各自的０，标准样品中ＭＭＡ、ＢＡ、Ｓｔ、ＨＰＡ、ＡＡ各ｉ，标准样品中ＭＭＡ、ＢＡ、Ｓｔ、ＨＰＡ、ＡＡ各０：乙酸丁酯质量，ｇ ）
取测定两次结果的算术平均值作为试样中ＭＭＡ、ＢＡ、Ｓｔ、ＨＰＡ、ＡＡ的测定结果。３．３ 方法的标准校正曲线和回收率
本方法以峰面积—浓度作标准校正曲线，具有良好的线性关系，峰面积—浓度回归方程的相关系数Ｒ值均大于０．９９，故可以采用外标法进行样品中残余单体含量的测定。ＦＩＤ检测器对丙烯酸树脂中各个残余单体的响应值比较灵敏，检出限低，为１０μｇ／ｋｇ，回收率为８９％～１１２％。
４ 结 语
（１）本方法适用于丙烯酸树脂和改性丙烯酸树脂中残余单体的检测。
（２）采用此方法具有快速、简便等优点。（３）在本方法中，对于谱柱的选择很关键，只要能够使丙烯酸树脂中的各种残余单体得到有效分离的谱柱均可采用。实验条件根据不同仪器、不同谱柱而有所变化。
收稿日期 ２００５－１１－０８
SUMMARIES
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