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高效液相色谱法测定水性涂料中甲醛含量的方法改进

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通过对GB/T 34683-2017方法中的DNPH衍生化试剂的配制方法、样品的衍生化处理、流动相试剂及洗脱程序的改进后,本方法的标准曲线相关系数为0.99976,色谱图中DNPH试剂峰型未出现双峰,方法检出限为0.12 mg/kg(以3倍标准偏差计算),其重现性:5 mg左右样品的两结果绝对偏差0.35 mg/kg、30 mg左右样品的两结果绝对偏差为0.6236 mg/kg、>30 mg样品的两结果绝对偏差为1.6553%,其再现性:5 mg左右样品两结果平均值的绝对偏差为0.1246 mg/kg、30 mg左右样品的两结果平均值的绝对偏差为0.1812 mg/kg、>30 mg样品两平均值结果绝对偏差与平均值的比值为0.3291%,加标回收率为96.2832,结果都优于GB/T 34683-2017,试验过程更简捷,从而使GB/T 34683-2017方法的时效性、简便性、准确性等方面得到了优化和改进.
Improved Method for Determination of Formaldehyde in Waterborne Coatings by High Performance Liquid Chromatography
After improving the preparation method of DNPH derivatization reagent,sample derivatization treatment,mobile phase reagent and elution procedure in GB/T 34683-2017 method,the correlation coefficient of the standard curve of this method is 0.99976,and the peak type of DNPH reagent does not appear double peaks in the chromatogram.The detection limit of the method was 0.12 mg/kg(calculated by 3 times standard deviation),and its reproducibility was as follows:the absolute deviation between the two results of about 5 mg sample was 0.35 mg/kg,the absolute deviation between the two results of about 30 mg sample was 0.6236mg/kg,and the absolute deviation between the two results of>30 mg sample was 1.6553%.Its reproducibility was as follows:The absolute deviation of the mean value of the two results was 0.1246 mg/kg for samples about 5 mg,0.1812 mg/kg for samples about 30 mg,0.3291%for samples>30mg,and the recovery rate was 96.2832.The results are better than GB/T 34683-2017,and the test process is more simple,so that the timeliness,simplicity and accuracy of GB/T 34683-2017 method have been optimized and improved.

DNPH derivatizationpre-treatmentmobile phase reagent and elution procedureimprovement

陈竹青、党增超、黄祝华、赵孝佳

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南京市产品质量监督检验院(南京市质量发展与先进技术应用研究院),江苏南京 210019

上海鼎泰匠芯科技有限公司,上海 201306

DNPH衍生化 前处理 流动相试剂及洗脱程序 改进

南京市市场监督管理局科技项目

Kj2022012

2024

化工设计通讯
湖南化工医药设计院

化工设计通讯

影响因子:0.126
ISSN:1003-6490
年,卷(期):2024.50(10)