顶空气相色谱-质谱法测定橡胶防老剂4020中的甲基异丁基酮和苯胺
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摘要
通过优化不同的平衡条件,建立了顶空气相色谱-质谱法测定防老剂4020中甲基异丁基酮和苯胺的方法。结果表明:在称样量为0. 5 g、顶空自动进样器的平衡温度为160℃、平衡时间为90 min的条件下,甲基异丁基酮和苯胺质量浓度线性关系良好,相关因数分别为0. 995和0. 989;方法检出限均为1 mg·kg~(-1);回收率为90%～110%,相对标准偏差为4. 4%～8. 0%。
The method for the determination of methyl isobutyl ketone and aniline in antioxidant 4020 by head space gas chromatography-mass spectrometry was established through optimizing different equilibrium conditions. The results showed that when the amount of sample was 0. 5 g,the equilibrium temperature of headspace autosampler was 160 ℃ and the balance time was 90 min,good linearity in a mass concentration range of methyl isobutyl ketone and aniline could be obtained,and the regression coefficients were 0. 995 and0. 989,respectively. The detection limit of the method was all 1 mg·kg~(-1),the recovery was 90%～110%,and the relative standard deviation was 4. 4%～8. 0%.
The method for the determination of methyl isobutyl ketone and aniline in antioxidant 4020 by head space gas chromatography-mass spectrometry was established through optimizing different equilibrium conditions. The results showed that when the amount of sample was 0. 5 g,the equilibrium temperature of headspace autosampler was 160 ℃ and the balance time was 90 min,good linearity in a mass concentration range of methyl isobutyl ketone and aniline could be obtained,and the regression coefficients were 0. 995 and0. 989,respectively. The detection limit of the method was all 1 mg·kg~(-1),the recovery was 90%～110%,and the relative standard deviation was 4. 4%～8. 0%.
引文
[1]陈慧.防老剂4020-80在全钢载重子午线轮胎胎面胶中的应用[J].橡胶科技,2013,11(7):32-35.
[2]惠炳国,王爱萍,王振太,等.优化型防老剂4020在全钢载重汽车子午线轮胎胎冠胶中的应用研究[J].橡胶科技市场,2010,8(17):11-14.
[3]梁克民,王凤娟,潘世伟.常压合成防老剂4020的工业生产工艺[J].合成橡胶工业,2003,26(6):339-341.
[4]朱书魁,郭旭东,王海波.橡胶防老剂4020/4010NA及中间体合成技术[J].沈阳化工,1999,3:30-32.
[5]袁俊盛.新型橡胶防老剂4020[J].合成橡胶工业,1982,5(2):72-73.
[6]王超,吕怡兵,滕恩江,等.超高压液相色谱荧光检测法快速测定水中痕量苯胺与联苯胺[J].分析测试学报,2013,32(1):32-37.
[7]薛科社,董发昕.高效液相色谱-荧光检测法测定环境水中的苯胺和苯酚[J].分析试验室,2004,23(9):36-38.
[8]邹玉林,陈勇,吕桂宾,等.液相色谱-质谱法测定水中的苯胺[J].化学研究与应用,2011,23(5):649-651.
[9]贺德春,赵波,唐才明,等.液相色谱-串联质谱法快速测定水及鱼肉中的苯胺[J].色谱,2014,32(9):926-929.
[10]蒋凝.气相色谱法测定防老剂4020的纯度[J].化学工业与工程技术,2007(S1):295-297.
[2]惠炳国,王爱萍,王振太,等.优化型防老剂4020在全钢载重汽车子午线轮胎胎冠胶中的应用研究[J].橡胶科技市场,2010,8(17):11-14.
[3]梁克民,王凤娟,潘世伟.常压合成防老剂4020的工业生产工艺[J].合成橡胶工业,2003,26(6):339-341.
[4]朱书魁,郭旭东,王海波.橡胶防老剂4020/4010NA及中间体合成技术[J].沈阳化工,1999,3:30-32.
[5]袁俊盛.新型橡胶防老剂4020[J].合成橡胶工业,1982,5(2):72-73.
[6]王超,吕怡兵,滕恩江,等.超高压液相色谱荧光检测法快速测定水中痕量苯胺与联苯胺[J].分析测试学报,2013,32(1):32-37.
[7]薛科社,董发昕.高效液相色谱-荧光检测法测定环境水中的苯胺和苯酚[J].分析试验室,2004,23(9):36-38.
[8]邹玉林,陈勇,吕桂宾,等.液相色谱-质谱法测定水中的苯胺[J].化学研究与应用,2011,23(5):649-651.
[9]贺德春,赵波,唐才明,等.液相色谱-串联质谱法快速测定水及鱼肉中的苯胺[J].色谱,2014,32(9):926-929.
[10]蒋凝.气相色谱法测定防老剂4020的纯度[J].化学工业与工程技术,2007(S1):295-297.