旋流气液分离-电感耦合等离子体原子发射光谱法测定有机脱碳液中总无机碳  

Determination of total inorganic carbon in organic decarbonization liquid by inductively coupled plasma atomic emission spectrometry with swirling gas-liquid separation

作　　者：麻安菊 成勇[1] 袁金红[1] 何其平[1] 魏芳[1] MA Anju;CHENG Yong;YUAN Jinhong;HE Qiping;WEI Fang(Pangang Group Research Institute Co.,Ltd.,Panzhihua 617067,China)

机构地区：[1]攀钢集团研究院有限公司,四川攀枝花617067

出　　处：《冶金分析》2025年第3期44-50,共7页Metallurgical Analysis

摘　　要：以醇胺等有机脱碳液捕集吸附工业烟气中二氧化碳是碳达标的主流技术之一,准确测定以无机碳酸盐形态存在的总无机碳含量,对于脱碳液性能评价与捕集工艺优化至关重要,而有机基体共存会严重干扰测定结果。本文利用电感耦合等离子体原子发射光谱仪(ICP-AES)的雾化传输进样系统原有部件,构建一套可将无机碳从有机溶液中分离出来的旋流气液分离装置,通过在线混合盐酸和有机脱碳液,促使无机碳转化为气态二氧化碳而被测定,从而建立电感耦合等离子体原子发射光谱法测定有机脱碳液中总无机碳含量的方法。考察了反应池长度、载气流速、盐酸浓度等对无机碳测定的影响以及气液分离效果,确定了测定条件:反应池为长度6 cm,载气流速为0.3 L/min,反应剂为盐酸(1+1),分析谱线为C 193.030 nm。结果表明,以二乙醇胺(DEA)为介质绘制校准曲线,待测无机碳质量浓度在10~720 mg/L内,线性相关系数不小于0.999,检出限为0.039 mg/L。按照实验方法测定吸收过二氧化碳的醇胺溶液样品中总无机碳含量,结果的相对标准偏差(RSD,n=10)不大于5.6%,回收率为98%~105%。方法有效解决了有机基体对无机碳检测的干扰问题,满足快速分析多种工业有机脱碳液中无机碳的需要。The capture and adsorption of carbon dioxide in industrial flue gas by organic decarbonization liquid such as alkanolamine is one of the mainstream technologies for carbon compliance.The accurate determination of total inorganic carbon content in the form of inorganic carbonate is crucial for the performance evaluation of decarbonization liquid and the optimization of capture process,while the coexistence of organic matrix will seriously interfere with the determination results.In this study,a swirling gas-liquid separation device for separating inorganic carbon from organic solution was constructed using the original part of atomization transfer system of inductively coupled plasma atomic emission spectrometer(ICP-AES).By online mixing of hydrochloric acid with organic decarburization liquid,the inorganic carbon was converted into gaseous carbon dioxide and then determined.Consequently,a method for the determination of total inorganic carbon in organic decarburization liquid by inductively coupled plasma atomic emission spectrometry was established.The influence of reactor length,carrier gas flow rate and hydrochloric acid concentration on the determination of inorganic carbon and the gas-liquid separation effect was investigated.The optimized determination conditions were obtained as follows:the reaction cell length was 6 cm,the carrier gas flow rate was 0.3 L/min,the reaction agent was hydrochloric acid(1+1),and the analytical line was C 193.030 nm.The calibration curve was drawn with diethanolamine(DEA)as the medium.The results showed that the linear correlation coefficient was higher than 0.999 when the mass concentration of inorganic carbon was in the range of 10-720 mg/L.The limit of detection was 0.039 mg/L.The content of total inorganic carbon in alkanolamine solution sample after absorbing carbon dioxide was determined according to the experimental method.The relative standard deviation(RSD,n=10)was not more than 5.6%,and the recoveries were 98%-105%.The method effectively solved the interference proble

关 键 词：旋流气液分离 电感耦合等离子体原子发射光谱法(ICP-AES) 有机脱碳液 无机碳 

分 类 号：O657.31[理学—分析化学]