用于离子色谱系统淋洗液中CO2脱除的气液分离器设计与应用

doi:10.3724/SP.J.1123.2024.03021

摘要/Abstract

摘要：

设计了一种可用于脱除离子色谱(IC)系统淋洗液中CO₂的气液分离器(GLS)。首先将微孔中空纤维聚丙烯管(PP-T)内插到内径适配的聚四氟乙烯管(PTFE-T)中,形成双套管结构并缠绕成螺旋形;随后将PP-T和PTFE-T的两端分别固定于配备了三通接头的两个水平接口处,将再生液管路固定在配备了三通接头的垂直臂接口处。当碳酸根淋洗液从上游抑制器流入PP-T内部时,经抑制作用后的碳酸溶液会分解产生CO₂气体,这些气体随后通过PP-T逸出,并进入位于PP-T与PTFE-T之间环状空间内的流动吸收液中,从而实现CO₂的持续、有效脱除。实验优化了GLS的制作条件和操作条件,包括PP-T的长度、PTFE-T的内径、操作温度和吸收液的种类、浓度及流速等。实验结果表明,将40 mmol/L的KOH溶液作为吸收液时,在淋洗液流速为1 mL/min的情况下,CO₂的脱除效率可达98%以上;较高的操作温度有助于提高CO₂的脱除效率并降低基线噪声,本实验优化后的操作温度为40 ℃。将该GLS应用于碳酸根淋洗液的IC系统,在使用1.8 mmol/L K₂CO₃-3.2 mmol/L KHCO₃(1∶1, v/v)混合淋洗液时,背景电导信号从未使用GLS的41.6 mV降低至使用GLS后的5.5 mV;以150 μmol/L常见阴离子(F^-、Cl^-、 $NO 2 -$ 、Br^-、 $NO 3 -$ 、 $SO 4 2 -$ )混合标准溶液为标样,使用GLS后的信噪比(SNR)得到了明显提升(6.0~11.8倍)。此外,该GLS还可用于脱除氢氧根淋洗液体系下大体积样品中的CO₂( $CO 3 2 -$ 的峰面积下降了约80%),降低样品中 $CO 3 2 -$ 对其他阴离子分离产生的干扰。

关键词: 离子色谱, 气液分离器, CO₂脱除, 阴离子分析, 抑制器

Abstract:

A gas-liquid separator (GLS) for the removal of carbon dioxide in the eluent of an ion chromatography (IC) system was developed. Firstly, the microporous hollow fiber polypropylene tube (PP-T) was inserted into the polytetrafluoroethylene tube (PTFE-T) with suitable inner diameter to form a double casing structure and wound into a spiral shape. Each terminal of the PP-T is 3 cm longer than that of the PTFE-T. Then the terminals of PP-T and PTFE-T were fixed respectively on two horizontal joints equipped with tee joints, and the regenerated liquid pipeline was fixed on a vertical arm interface equipped with tee joints. When the carbonate eluent flows into PP-T from the upstream suppressor, the inhibited carbonate solution will decompose and produce CO₂, which then escapes through PP-T and enters the flowing absorption solution located in the annular space between PP-T and PTFE-T, so as to achieve continuous and effective CO₂ removal. The production conditions and operating conditions of GLS were optimized, including the length of PP-T, the inner diameter of PTFE-T, the operating temperature, the type, concentration and flow rate of the absorption solution. The experimental results show that when 40 mmol/L potassium hydroxide solution is used as absorption solution, the removal efficiency of CO₂ can reach more than 98% at the flow rate of 1 mL/min. Higher operating temperature is helpful to improve the removal efficiency of CO₂ and reduce the baseline noise. The optimized operating temperature in this study was 40 ℃. When applying this GLS to the IC system for carbonate eluent, using a mixed eluent of 1.8 mmol/L potassium carbonate-3.2 mmol/L potassium bicarbonate (1∶1, v/v), the background conductance signal decreased from 41.6 mV without GLS to 5.5 mV after using GLS. Using a mixed standard solution of common anions (F^-、Cl^-、 $NO 2 -$ 、Br^-、 $NO 3 -$ 、 $SO 4 2 -$ ) at 150 μmol/L as the reference sample, the signal-to-noise ratio (SNR) after applying the GLS has been significantly improved by a factor of 6.01 to 11.8 times. In addition, the GLS can also be used to remove CO₂ from large volume samples in hydroxide eluent system, reducing the interference of $CO 3 2 -$ on the separation of other anions.

Key words: ion chromatography (IC), gas-liquid separator (GLS), carbon dioxide removal, anion analysis, suppressor

中图分类号:

O658

彭勇涵, 唐婧雯, 李怡桦, 章飞芳, 杨丙成. 用于离子色谱系统淋洗液中CO₂脱除的气液分离器设计与应用[J]. 色谱, 2025, 43(4): 382-387.

PENG Yonghan, TANG Jingwen, LI Yihua, ZHANG Feifang, YANG Bingcheng. Design and application of a gas-liquid separator for the removal of carbon dioxide in the eluent of an ion chromatography system[J]. Chinese Journal of Chromatography, 2025, 43(4): 382-387.

图/表 5

图1 用于脱除CO2的GLS结构示意图

Fig. 1 Structure diagram of gas liquid separator (GLS) E-IN: eluent inlet; E-OUT: eluent outlet; R-IN: regenerated fluid inlet; W-OUT: waste outlet; PP-T: polypropylene tube; PTFE-T: polytetrafluoroethylene tube.

图2 PP-T长度对(a)背景电导信号、(b)SNR及塔板数的影响

Fig. 2 Effects of PP-T length on (a) background conductance signal, (b) signal-to-noise (SNR) and plate number Chromatography column: TSKgel SuperIC-AZ (150 mm×4.6 mm); eluent: 10 mmol/L potassium carbonate solution (flow rate 0.8 mL/min); injection volume: 25 μL; suppression current: 50 mA; absorption solution: 40 mmol/L potassium hydroxide solution (flow rate 1 mL/min); detector: homemade conductivity detector.

图3 KOH溶液的流速对CO2脱除效率及噪声的影响

Fig. 3 Effect of flow rate of potassium hydroxide solution on CO2 removal efficiency and noise PP-T length: 2 m; chromatography column: TSKgel SuperIC-AZ (150 mm×4.6 mm); eluent: 10 mmol/L potassium carbonate solution (flow rate 0.8 mL/min); injection volume: 25 μL; suppression current: 50 mA; absorption solution: 40 mmol/L potassium hydroxide solution; detector: homemade conductivity detector.

图4 GLS应用于碳酸根淋洗液体系的效果

Fig. 4 Effect of GLS applied to carbonate eluent system PP-T length: 2 m; chromatography column: TSKgel SuperIC-AZ (150 mm×4.6 mm); eluent: 10 mmol/L potassium carbonate solution (flow rate 0.8 mL/min); injection volume: 25 μL; suppression current: 50 mA; absorption solution: 40 mmol/L potassium hydroxide solution (flow rate 1 mL/min); detector: homemade conductivity detector.

图5 GLS应用于氢氧根淋洗液体系的效果

Fig. 5 Effect of GLS applied to hydroxide eluent system a. PP-T length: 2 m; chromatography column: HS-5A-PS (250 mm×4.0 mm); eluent: 20 mmol/L potassium hydroxide solution (flow rate 0.7 mL/min); injection volume: 200 μL; suppression current: 50 mA; absorption solution: suppressor regenerant; sample mass concentration (mg/L): Cl-(0.4), dichloroacetic acid (DCA) (0.4), N O 2 -(0.5), Cl O 3 -(1.0), Br-(0.25), N O 3 -(0.66), trichloroacetic acid (TCA) (0.5), S O 4 2 -(0.5); detector: homemade conductivity detector. b. PP-T length: 2 m; chromatography column: Thermo IonPacTM AS18 (250 mm×4.0 mm); eluent: 18 mmol/L potassium hydroxide solution generated by electrodialytic eluent generator (EDG) (flow rate 1 mL/min); suppression current: 45 mA; absorption solution: suppressor regenerant; injection volume: 1 mL; sample mass concentration: 1 mmol/L lithium hydrate solution containing 50 μg/L anion mixture of F-, Cl-, NO 2 -, SO 4 2 -, NO 3 -; detector: TOSOH ion chromatography conductivity detector.

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用于离子色谱系统淋洗液中CO₂脱除的气液分离器设计与应用

Design and application of a gas-liquid separator for the removal of carbon dioxide in the eluent of an ion chromatography system

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