超声萃取-气相色谱法测定刹车片摩擦层中游离苯酚  

Determination of free phenol in friction layer of brake pad by gas chromatography with ultrasonic extraction

作　　者：余建龙 刘健斌 李全忠 卢焯冬 房兆龙 吴长俊 YU Jianlong;LIU Jianbin;LI Quanzhong;LU Zhuodong;FANG Zhaolong;WU Changjun(Guangzhou Customs District Technology Center,Guangzhou 510623,China;Huangpu Customs District Technology Center,Guangzhou 510700,China;China Certification&Inspection Group Guangdong Co.,Ltd.,Guangzhou 510623,China)

机构地区：[1]广州海关技术中心,广东广州510623 [2]黄埔海关技术中心,广东广州510700 [3]中国检验认证集团广东有限公司,广东广州510623

出　　处：《冶金分析》2024年第6期44-48,共5页Metallurgical Analysis

基　　金：国家重点研发计划项目(2021YFF0602603)。

摘　　要：刹车片摩擦层中游离苯酚会挥发进入空气中从而污染人们的生活环境,因此需要准确测定并控制其含量。将样品装进洁净的冷冻粉碎钢瓶内,通过液氮冷冻粉碎为粒径0.075~0.150 mm的粉末状固体,称取0.5~1.0 g粉末状固体,用乙醇超声萃取30 min,定容后取上层清液,用0.45μm滤膜过滤,采用HP-INNOWax毛细管色谱柱进行分离后用气相色谱法进行测定,实现了气相色谱法对刹车片摩擦层中游离苯酚的测定。实验表明,游离苯酚在2.0~200 mg/L质量浓度范围内与其对应的色谱峰面积呈线性关系,线性相关系数为0.9995,方法定量限为10 mg/kg。按照实验方法测定4个刹车片摩擦层样品中游离苯酚的含量,结果表明,游离苯酚测定结果的相对标准偏差(RSD,n=6)不大于3%。在样品中分别添加5.0、10.0、30.0 mg/L苯酚标准工作液进行加标回收试验,回收率为86%~107%。Free phenol in the friction layer of brake pads will volatilize into the air and pollute people's living environment,so it is necessary to accurately determine and control its content.After the sample was transferred into a clean cryogenic grinding steel cylinder,it was frozen and pulverized into a powdered solid with particle size of 0.075-0.150 mm by liquid nitrogen.0.5-1.0 g of solid powder was weighed and treated by ultrasonic extraction for 30 min with ethanol.After dilution to the mark,the supernatant liquor was filtered with 0.45μm membrane.Then it was separated with HP-INNOWax capillary column and determined by gas chromatography.Consequently,the determination of free phenol in the friction layer of brake pads was realized by gas chromatography.The results showed that the concentration of free phenol in range of 2.0-200 mg/L had a linear relationship with its corresponding chromatographic peak area.The linear correlation coefficient was 0.9995,and the limit of quantification of method was 10 mg/kg.The contents of free phenol in 4 friction layer samples of brake pad were determined according to the proposed method.The results showed that the relative standard deviations(RSD,n=6)of determination results of free phenol were less than 3%.5.0,10.0 and 30.0 mg/L of phenol standard working solution was added into sample for recovery tests.The recoveries were between 86% and 107%.

关 键 词：气相色谱法 毛细色谱柱 刹车片 摩擦层 游离苯酚 

分 类 号：O657.71[理学—分析化学] U463.55[理学—化学]