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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
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- DOI:
- 作者:
- 荣丽丽，王 磊，靳丽丽，沈 刚
Rong Lili，Wang Lei，Jin Lili，Shen Gang
- 作者单位:
- 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
PetroChina Petrochemical Research Institute Daqing Chemical Engineering Research Center，Daqing 163714，China
- 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
high-temperature melting；ICP-AES；polyethylene；polypropylene；silicon
- 摘要:
- 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（Li2B4O7 ）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。Abstract：According to standard T / CPCIF 0096-2021, the determination of silicon in polyethylene and polypropylene usinghigh-temperature melting inductively coupled plasma atomic emission spectroscopy. By adding lithium tetraborate as meltingreagent into the ashed samples of polyethylene and polypropylen at 975 ℃ to prepare the molten glass, and then dissolved in tartaricacid and hydrochloric acid at low temperature to obtain the solution to be tested.Si 261.611 nm was selected as the optimum spectralline. The calbbration curve for silicon, ranged from 1.0 mg/L to 10.0 mg/L, using matrix matching method.The limit of detection was0.25 mg / L. The precision test was conducted by selecting five samples. All the relative standard deviation （RSD，n=7）ofdetermination were 1.0%~3.0%, and the standard recoveries range between 95% and 105%. Results the method showed goodprecision and high accuracy.Both melting-acid dissolution method and microwave digestion method could effectively dissolved thesample completely. Compared with the microwave digestion method, melting-acid dissolution method has more advantages todetermin silicon for minimal SiF4 volatilization loss during the microwave digestion process.