基于化学沉淀的水性建筑涂料游离甲醛含量快速检测体系的研究  

Study on rapid detection system of free formaldehyde content in waterborne architectural coatings based on chemical precipitation

作　　者：霍炜江 沈文洁 彭速标 肖前 岳大磊 HUO Wei-jiang;SHEN Wen-jie;PENG Su-biao;XIAO Qian;YUE Da-lei(Guangzhou Customs District Technology Center,Gangzhou 510623,China)

机构地区：[1]广州海关技术中心,广东广州510623

出　　处：《化学研究与应用》2022年第7期1690-1696,共7页Chemical Research and Application

基　　金：中国海关总署科技项目(2020HK237)资助。

摘　　要：建立了基于化学沉淀的水性建筑涂料游离甲醛含量快速检测体系,开发了一套水性涂料样品前处理方案。通过亚铁氰化钾与乙酸锌所生成的沉淀物亚铁氰化锌对涂料进行澄清净化,以偏重亚硫酸钠溶液对样品中游离甲醛进行提取,过滤后加入氢氧化钾、4-氨基-3-肼基-5-巯基-1,2,4-三氮唑(AHMT)及高碘酸钾将甲醛缩合氧化成紫红色的6-疏基-5-三氮杂茂[4,3-b]-S-四氮杂苯(Ⅲ),利用紫外-可见分光光度计测定产物的吸光度值。该方法游离甲醛的线性范围为0.50μg~64μg,r^(2)=0.9990,定量限为2.5 mg·kg^(-1)。以质控标样进行试验,相对偏差为1.5%。以4种水性涂料进行重复性与回收率试验,相对标准偏差在1.8%~8.8%的范围内,三个浓度水平的回收率在88%~105%的范围内。In this study,a rapid detection system of free formaldehyde in waterborne architectural coatings based on chemical precipitation was established,and a new scheme for sample pretreatment of waterborne coatings was also developed.The coatings would be clarified and purified by the precipitate zinc ferrocyanide formed by potassium ferrocyanide and zinc acetate,free formaldehyde in coatings could be extracted with sodium metabisulfite,after filtration of the extract,potassium hydroxide,4-Amino-3-hydrazino-1,2,4-triazol-5-thiol(AHMT)and potassium periodate were added to condense and oxidize the free formaldehyde into 6-sparse-5-triazene[4,3-b]-s-tetraazabenzene(Ⅲ).The absorbance value of the product could be determined by ultraviolet-visible spectrophotometer.Linearity range of free formaldehyde determination was between 0.50μg~64μg,and the linear correlation coefficient(r^(2))was 0.9990 with detection limit of 2.5 mg·kg^(-1).The accuracy was tested by quality control sample and the relative deviation was 1.5%.In the repeatability and recovery test of four kinds of waterborne architectural coatings,the relative standard deviation was in the range of 1.8%~8.8%,and the recovery of three concentration levels was in the range of 88%~105%.

关 键 词：水性建筑涂料 游离甲醛 化学沉淀 快速测定 

分 类 号：O652.3[理学—分析化学]