高温熔融ICP-AES测定PE、PP中的Si含量  

Determination of silicon in PE and PP by high temperature meltinginductively coupled plasma atomic emission spectrometry

作　　者：荣丽丽 王磊[1] 靳丽丽 沈刚 Rong Lili;Wang Lei;Jin Lili;Shen Gang(PetroChina Petrochemical Research Institute Daqing Chemical Engineering Research Center,Daqing 163714,China)

机构地区：[1]中国石油石油化工研究院大庆化工研究中心,黑龙江大庆163714

出　　处：《炼油与化工》2024年第3期34-38,共5页Refining And Chemical Industry

摘　　要：依据标准T/CPCIF 0096-2021,采用高温熔融—电感耦合等离子体原子发射光谱法(ICP-AES)测定聚乙烯(PE)、聚丙烯(PP)中的硅(Si)含量。四硼酸锂(Li_(2)B_(4)O_(7))作熔融试剂,975℃对PE、PP灰化后样品进行高温熔融处理,酒石酸—盐酸(HCl)于低温下对熔融后的玻璃液进行溶解,获得待测溶液。选择261.611 nm为Si元素最佳分析谱线,利用基体匹配的方法制备Si标准溶液系列,曲线范围在1.00~10.00 mg/L,Si检出限为0.25 mg/kg。选取5个样品开展精密度试验,RSD结果均为1.0%~3.0%;采用熔融法处理,获得加标回收率在95%~105%之间,精密度好、准确度高。对比了高温熔融和微波消解法,此2种方法均能较好的将样品完全溶解,其中微波消解法过程存在少量SiF4挥发损失,因此Si元素的处理上使用高温熔融法更有优势。According to standard T/CPCIF 0096-2021,the determination of silicon in polyethylene and polypropylene using high-temperature melting inductively coupled plasma atomic emission spectroscopy.By adding lithium tetraborate as melting reagent into the ashed samples of polyethylene and polypropylen at 975℃to prepare the molten glass,and then dissolved in tartaric acid and hydrochloric acid at low temperature to obtain the solution to be tested.Si 261.611 nm was selected as the optimum spectral line.The calbbration curve for silicon,ranged from 1.0 mg/L to10.0 mg/L,using matrix matching method.The limit of detection was 0.25 mg/L.The precision test was conducted by selecting five samples.All the relative standard deviation(RSD,n=7)of determination were 1.0%~3.0%,and the standard recoveries range between 95%and 105%.Results the method showed good precision and high accuracy.Both melting-acid dissolution method and microwave digestion method could effectively dissolved the sample completely.Compared with the microwave digestion method,melting-acid dissolution method has more advantages to determin silicon for minimal SiF4 volatilization loss during the microwave digestion process.

关 键 词：高温熔融 电感耦合等离子体原子发射光谱法 PE PP Si 

分 类 号：O657.31[理学—分析化学]