离子色谱法测定纺织浆料中痕量N-(2-羟乙基)乙二胺

IC Determination of Trace Amount of N-(2-Hydroxyethyl)-ethylene Diamine in Textile Sizing Agent

应用离子色谱法测定了纺织浆料中痕量的N-(2-羟乙基)乙二胺(HEEDA)。样品(1.0g)加水定容至25mL并超声分散40min,离心分离,取上清液,经过滤后再通过OnGuard RP柱除去其中的芳香染料等大分子有机物后,进样25μL,经Ionpac CS17阳离子交换柱,并用8mmol·L-1硫酸溶液作为流动相进行分离。用抑制电导检测器检测。HEEDA的质量浓度在0.1~100mg·L-1范围内与其峰面积值呈线性关系,检出限(3S/N)为0.025mg·L-1。按试验方法对50mg·L-1 HEEDA标准溶液重复5次测定,测定值的相对标准偏差为0.71%。以两个阳性样品作基体,用标准加入法进行回收试验,测得回收率在95.4%~104%之间。

IC was applied to the determination of trace amounts of N-(2-hydroxyethyl)-ethylene diamine(HEEDA)in textile sizing agent.The sample(1.0g)was mixed and made up to 25 mL with water,and then dispersed ultrasonically for 40 min.After centrifuged,the supernatant was taken and passed through OnGuard RP column to remove aromatic dyes and other macromolecular organic substances.An aliquot of 25μL of the sample solution was separated on Ionpac CS17 cationic exchange column with 8 mmol·L-1 H2SO4 solution as mobile phase.The suppressed conductivity detector was adopted in the IC determination.Linear relationship between values of peak area and mass concentration of HEEDA was kept in the range of 0.1to 100mg·L-1,with detection limit(3S/N)of 0.025mg·L-1.Repeatability was tasted on standard solution with 50mg·L-1 of HEEDA,value of RSD(n=5)found was 0.71%.Recovery was tested by standard addition method using 2positive samples of sizing agents,as matrixes,giving values of recovery in the range of 95.4%-104%.