间羟基-N,N-二乙基苯胺中Cl-的离子色谱法测定

采用离子色谱法测定间羟基-N,N-二乙基苯胺中残留氯离子,以Na2CO3/NaHCO3混合溶液为流动相,用IonPac AS14分析柱分离,实验结果较理想。该方法操作简便,结果准确。

萃取分离-离子色谱法测定间羟基-N,N-二乙基苯胺中的无机阴离子

建立了检测常用化工原料间羟基-N,N-二乙基苯胺中无机阴离子(F-、Cl-、NO3-和SO42-)含量的萃取分离-离子色谱分析方法。方法以甲苯为溶剂溶解间羟基-N,N-二乙基苯胺,用水相萃取分离得到其中的无机阴离子F-、Cl-、NO3-和SO42-等;色谱柱采用Metrosep A supp 5型阴离子分离柱,流动相为3.2 mmol/L Na2CO3与1.0 mmol/L NaHCO3的混合液,流速0.7 mL/min。结果表明:F-、Cl-、NO3-和SO42-的线性关系分别为y=1.2036x+1.0703(r=0.9999)、y=1.3999x-0.2531(r=0.9999)、y=2.6612x-0.9482(r=1.0000)、y=1.9337x+0.0719(r=0.9999);平均回收率分别为F-101.6%(RSD 5.92%),Cl-107.6%(RSD 4.82%),NO3-106.9%(RSD 3.08%),SO42-95.17%(RSD 3.32%);检出限分别为:F-0.003 mg/L、Cl-0.005 mg/L、NO3-0.016 mg/L和SO42-0.010 mg/L。该方法简便、快速、灵敏度高,具有较强的实用价值。

Synthesis and characterization of 2-hydroxy-N-methyl-N-phenyl-acetamide

2-hydroxy N methyl N phenyl acetamide was synthesized by using N methylaniline, chloracetyl chloride, anhydrous sodium acetate and methanol through the acetylation, esterfication and ester interchange steps. The acetylation of N methylaniline with chloracetyl chloride, catalyzed by triethylamide with mole ratio n (C 6H 5NHCH 3)∶ n (ClCH 2C(O)Cl)∶ n (N(C 2H 5) 3)=1∶1.05∶1, the yield of 2 chloro N methyl N phenyl acetamide(Ⅰ) was 93.8%; Then the esterification of Ⅰ with anhydrous sodium acetate in the presence of phase transfer catalyst tetrabutyl ammonia bromide gave 97.3% yield of 2 acetoxyl N methyl N phenyl acetamide (Ⅱ); The ester interchange of with methanol catalyzed by potassium hydroxide gave 2 hydroxy N methyl N phenyl acetamide (Ⅲ) in 96.4% yield. And the total yield was 88.0%. IR and MS spectroscopy of products were analyzed and their characteristic peaks were assigned. Combining the results of elemental analysis, the molecular structure of Ⅰ, Ⅱ and Ⅲ was identified.