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投稿时间：2024-01-20 修订日期：2024-01-22
投稿时间：2024-01-20 修订日期：2024-01-22
中文摘要: 稀土元素会对橡胶的性能造成影响，需加强监控。本实验利用微敞开石墨消解技术结合等离子体质谱仪,构建了测定天然橡胶制品中16种稀土元素含量的方法,并系统分析了消解试剂、消解温度以及消解时间等因素对检测分析的影响,对设备工作功率、步距深度、冷却气流速、辅助气流速、雾化气流速等质谱参数进行优化筛选,利用在线内标手段校正了基体效应和信号漂移等问题。结果表明,微敞开石墨消解橡胶制品的较优处理条件如下:以6 mLHNO3、1 mL HClO4和4 mLHF为消解试剂,采用三阶程序升温,消解最高温度至180 ℃，保温180 min。新建立的方法具有较低的检出限,稀土元素的检出限范围为0.0002-0.0011 mg/kg,方法回收率在71.1 %-90.9%之间,RSD在3.8%-9.2%之间,各元素的标准曲线线性关系良好。与传统方法相比,微敞开石墨消解技术操作简便,可按照设定程序自动完成消解全过程,无需单独赶酸,工作效率较高。本方法具有成本低、检测范围宽、处理效率高等优点,适用于橡胶制品中稀土元素的高通量检测。已应用于实际橡胶制品的检测分析,不同类型橡胶制品中的稀土元素含量各不相同。
中文关键词: 橡胶制品 电感耦合等离子体质谱仪 微敞开石墨消解 稀土元素
Abstract:Rare earth elements can have an impact on the performance of rubber, and monitoring needs to be strengthened.This experiment is based on the use of micro-open graphite digestion technology combined with plasma mass spectrometry in order to provide a research basis for the preparation and revision of standards for the detection of rare earth elements in rubber products. It established a method to determine the content of 16 rare earth elements in natural rubber products, and systematically analyzed the influence of factors such as digestion reagent, digestion temperature and digestion time on the detection and analysis. The mass spectrometry parameters, such as the working power of the equipment, sampling depth, cooling gas flow rate, auxiliary gas flow rate, and atomization gas flow rate, were optimized and screened, and the matrix effect and signal drift that occurred during the detection process were also corrected by using online internal standard means. It was shown that the micro-open graphite ablation of rubber products had the following optimal processing conditions: 6 mL HNO3, 1.5 mL HClO4 and 4 mL HF as the ablation reagents, and the third-order program was used to elevate the temperature, and the maximum temperature of the ablation was up to 180 ℃, and the heat preservation was carried out for 180 min. The new method established has a low detection limit, the detection limit of rare earth elements ranged from 0.0002-0.0011 mg/kg, the method recovery was between 71.1 % and 90.9%, the RSD was between 3.8 % and 9.2%, which obtained a good linear relationship to meet the requirements of detection experiments. Compared with the traditional pretreatment method, the micro-open graphite digestion technique is easy to operate, and it can automatically complete the whole process of digestion according to the set program, without the need to drive the acid separately, so the working efficiency is higher. This method has the advantages of short time-consumption, low cost, wide detection range and high processing efficiency, and it is suitable for the high-throughput detection of rare earth elements in rubber products. It has been applied to the detection and analysis of actual rubber products. Different types of rubber products have different contents of rare earth elements.
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基金项目:海南省自然科学基金(321QN0927、323QN289、423QN292)、中央级公益性科研院所基本科研业务费专项(1630122023012)。
引用文本：
潘晓威,梁耀辉,占国艳,潘政,陈淑贤,文典,叶剑芝.微敞开石墨消解-电感耦合等离子体质谱(ICP-MS)法测定橡胶制品中稀土元素含量[J].中国无机分析化学,2024,14(11):1581-1588.
panxiaowei,liangyaohui,zhanguoyan,panzheng,chenshuxian,wendian,yejianzhi.Determination of Rare Earth Elements Content in Rubber Products by Inductively Coupled Plasma Mass Spectrometry with Micro-Open Graphite Digestion[J].Chinese Journal of Inorganic Analytical Chemistry,2024,14(11):1581-1588.
潘晓威,梁耀辉,占国艳,潘政,陈淑贤,文典,叶剑芝.微敞开石墨消解-电感耦合等离子体质谱(ICP-MS)法测定橡胶制品中稀土元素含量[J].中国无机分析化学,2024,14(11):1581-1588.
panxiaowei,liangyaohui,zhanguoyan,panzheng,chenshuxian,wendian,yejianzhi.Determination of Rare Earth Elements Content in Rubber Products by Inductively Coupled Plasma Mass Spectrometry with Micro-Open Graphite Digestion[J].Chinese Journal of Inorganic Analytical Chemistry,2024,14(11):1581-1588.
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