基于联用扫描电镜-能谱法和红外光谱法测定氟树脂涂料中PVDF树脂含量  

Determination PVDF Resin Content in Fluorocarbon Resin Coatings Base on the Combination of Scanning Electron Microscopy-Energy Dispersive Spectroscopy and Infrared Spectroscopy

作　　者：黎军 罗家和 陈侣平 霍斯欣 沈宏林 Li Jun;Luo Jiahe;Chen Lvping;Huo Sixin;Shen Honglin(Guangdong Testing Institute of Product Quality Supervision,Guangzhou 510330,China)

机构地区：[1]广东产品质量监督检验研究院,广东广州510330

出　　处：《广东化工》2024年第15期149-150,178,共3页Guangdong Chemical Industry

摘　　要：建立使用扫描电子显微镜-能谱法(SEM-EDS)鉴定热熔型氟树脂(PVDF)涂料中氟元素,红外光谱法(IR)定量测定树脂中PVDF(聚偏二氟乙烯)树脂含量方法。在EDS中氟元素的X射线分析线Kα为0.677 KeV,而氧元素的Kα为0.525 KeV,故氧不干扰氟的鉴定,元素周期表中其他元素也不干扰氟的测定。氟碳树脂涂料的树脂由丙烯酸树脂和PVDF树脂构成,丙烯酸树脂IR特征峰(羰基)为1724 cm^(-1),PVDF的IR特征峰为874 cm^(-1),以这两个特征峰的吸光度比值与PVDF含量关系建立线性回归方程进行定量分析,得到方程为Y(吸光度比值)=-0.0274X(PVDF含量)+2.499,R^(2)=0.9932。由于不同型号丙烯酸树脂羰基含量不同,本文使用IR法对定量结果进行了修正。本文以氟树脂涂料的清面漆、有色底漆和有色面漆为例进行检测,结果为测定值与标准方法测定值相对误差小于2%。此联用方法适用于粉末、液态氟碳涂料检测。A method for identifying fluorine elements in hot-melt fluorocarbon resin(PVDF)coatings by scanning electron microscopy-energy dispersive spectroscopy(SEM-EDS)and quantitative determination of PVDF(polyvinylidene fluoride)resin content in resin by infrared spectroscopy(IR)was established.In EDS,the X-ray analysis line Kαof fluorine element is 0.677 KeV,while the Kαof oxygen element was 0.525 KeV,so oxygen didn’t interfere with the identification of fluorine,and other elements in the periodic table didn’t interfere with the determination of fluorine also.The resin of fluorocarbon resin paint was composed of acrylic resin and PVDF resin,and the IR characteristic peak(carbonyl)of acrylic resin was 1724 cm^(-1),and the IR characteristic peak of PVDF was 874 cm^(-1).The linear regression equation was obtained based on the relationship between the absorbance ratio of these two characteristic peaks and the PVDF content,and the equation was Y(absorbance ratio)=-0.0274 X(PVDF content)+2.499,R^(2)=0.9932.Due to the different carbonyl content of different acrylic resins,the quantitative results were modified using the IR method.In this paper,the clear topcoat,colored primer and colored topcoat of fluorocarbon resin were used as examples,and the results showed that the relative error between the quantitative value and the standard method measurement value was less than 2%.This combination method was suitable for the detection of powdered and liquid fluorocarbon resin coatings.

关 键 词：扫描电镜 能谱 红外光谱 PVDF树脂 

分 类 号：O6[理学—化学]