基于重氮化-偶合显色反应的纺织品中禁用偶氮染料快速定性筛选方法

利用芳香胺的重氮化-偶合显色反应原理，建立了纺织品中24种禁用芳香胺的快速定性筛选测定方法。样品经还原后，先用10mL叔丁基甲醚萃取，再用5mLHCl反萃取，达到净化和脱色的目的，HCl萃取液中加入0．05mLNaNO2，重氮化反应10min，滴加0．5mL氨基磺酸铵除去多余的NaNO2，加入1mL邻甲氧基苯酚与重氮盐偶联显色。根据萃取液是否显色，快速地对样品中是否含有禁用偶氮染料作出初步判断。方法的检出限低于15mg／kg，上千个实际样品测试无假阴性，假阳性概率为28％。本方法无需大型色谱仪器设备，与仪器测定方法相比，前处理时间缩短了约60％，节约了约90％的试剂费用。...

Full description

Saved in:
Bibliographic Details
Published in分析化学 Vol. 41; no. 7; pp. 1107 - 1110
Main Author 叶曦雯 牛增元 李引 张清智 高永刚 罗忻
Format Journal Article
LanguageChinese
Published 山东出入境检验检疫局,青岛,266002%山东出入境检验检疫局,青岛266002 2013
青岛科技大学环境与安全工程学院,青岛266042
Subjects
显色反应
禁用偶氮染料
纺织品
芳香胺
邻甲氧基苯酚
重氮化-偶合反应
Guaiacol
重氮化-偶合反应
邻甲氧基苯酚
Aromatic amines
Textile
Banned azo dyes
显色反应
Color reaction
禁用偶氮染料
芳香胺
Diazotization-coupling reaction
纺织品
Online AccessGet full text
ISSN0253-3820
DOI10.3724/SP.J.1096.2013.21063

Cover

More Information
Summary:利用芳香胺的重氮化-偶合显色反应原理，建立了纺织品中24种禁用芳香胺的快速定性筛选测定方法。样品经还原后，先用10mL叔丁基甲醚萃取，再用5mLHCl反萃取，达到净化和脱色的目的，HCl萃取液中加入0．05mLNaNO2，重氮化反应10min，滴加0．5mL氨基磺酸铵除去多余的NaNO2，加入1mL邻甲氧基苯酚与重氮盐偶联显色。根据萃取液是否显色，快速地对样品中是否含有禁用偶氮染料作出初步判断。方法的检出限低于15mg／kg，上千个实际样品测试无假阴性，假阳性概率为28％。本方法无需大型色谱仪器设备，与仪器测定方法相比，前处理时间缩短了约60％，节约了约90％的试剂费用。
Bibliography:Based on the principle of diazotization-coupling color reaction of aromatic amines, a rapid qualita- tive screening method for detecting 24 banned aromatic amines dyes in textile was developed. After reduction reaction, sample solutions were extracted with 10 mL t-butyl methyl ether and 5 mL hydrochloric acid respec- tively. Then 0.05 mL sodium nitrite was mixed into extract liquids and maintained for 10 min. To get rid of redundant sodium nitrite, O. 5 mL Ammonium sulfamate was added in. Thereafter 1 mL of guaiacol was added as color reagent. According to the condition of presence or absence of color-reaction, preliminary judgment of whether the textiles containing banned azo dyes could be done. The results showed that the detection limit of the method was less than 15 mg/kg. It met the requirements of the current regulation limits. The test results of more than 1000 actual sample showed that there was no false negative case of this method and false positive rate was 28%. Comparing with current testing means
ISSN:0253-3820
DOI:10.3724/SP.J.1096.2013.21063