气相色谱法快速测定常量DNBP含量
Rapid Determination of Macro Content of DNBP by Gas Chromatography
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- DOI:
- 作者:
- 魏盼荣，王雨薇，牛艺霖，张高杰，陈世龙
Wei Panrong, Wang Yuwei, Niu Yilin, Zhang Gaojie, Chen Shilong
- 作者单位:
- 中国石油兰州石化公司
PetroChina Lanzhou Petrochemical Company
- 关键词:
- DNBP；阻聚剂；气相色谱法；重复性；准确度
DNBP; polymerization inhibitor; gas chromatography; repeatability; accuracy
- 摘要:
- 摘要：DNBP是苯乙烯精馏常用阻聚剂，其加入量对于工艺控制至关重要。DNBP传统分析方法为酸碱滴定法，分析时间长，需消耗大量乙苯等有毒试剂，对人体危害大。通过对分析方法改进，采用气相色谱法建立了DNBP含量测定方法，可检测0.24%~75.00%范围含量。通过实验验证，DNBP的相对标准偏差为 0.13%~0.20%，加标回收率为 92.94%~107.59%，表明气相色谱法有较好的重复性和准确度。通过采用气相色谱法与酸碱滴定法测量结果进行 F检验和t检验，验证结果符合要求，表明2种方法测定结果无显著性差异，可用于原材料日常分析，为生产装置优化工艺条件提供数据支持。
Abstract: DNBP is a commonly used polymerization inhibitor in styrene distillation, and its dosage is of critical importance for processcontrol. The traditional analytical method for DNBP is acid-base titration, which is time-consuming and requires the consumption of alarge amount of toxic reagents such as ethylbenzene, posing significant health hazards to operators. By improving the analytical approach, agas chromatography (GC) method has been developed for determining the content of DNBP, capable of detecting concentrations within therange of 0.24% to 75.00%. Experimental validation demonstrates that the relative standard deviation (RSD) of DNBP measurements rangesfrom 0.13% to 0.20%, and the spiked recovery rates are between 92.94% and 107.59%, indicating that the gas chromatography methodoffers good repeatability and accuracy. F-tests and t-tests conducted on the measurement results obtained by gas chromatography andacid-base titration show that the validation results meet the requirements, revealing no significant differences between the two methods.Therefore, this method can be applied to routine analysis of raw materials, providing data support for optimizing process conditions inproduction facilities.