Simultaneous determination of eight organic amines in desulfurization solution by ion chromatography

doi:10.3724/SP.J.1123.2023.09024

Abstract

Abstract:

The applications of organic-amine desulfurization have steadily increased owing to its high efficiency, low cost, and low energy consumption. Different proportions of organic amines exert different effects on sulfur dioxide removal. Therefore, the accurate determination of different organic amines in the desulfurization solution is of great importance. The ion-chromatographic method for the detection of organic amines does not require a derivatization step, has simple pretreatment procedures, and allows for the simultaneous determination of many types of organic amines. In this study, a method based on ion chromatography was developed for the simultaneous determination of ethanolamine (MEA), diethylethanolamine (DEEA), n-methyldiethanolamine (MDEA), 2-amino-2-methyl-1-propanol (AMP), hydroxyethylethylenediamine (AEEA), piperazine (PZ), n-hydroxyethylpiperazine (HEPZ), and diethylenetriamine (DETA). The separation efficiency of the eight organic amines in different types of columns, leaching solutions, and column temperatures were compared. The determination was performed using an IonPac CS17 column with column temperature of 35 ℃ and gradient leaching with methyl sulfonic acid (MSA) solution via the inhibition conductance method. Samples of the desulfurization solution were analyzed using ultrapure water filtered through a 0.22 μm nylon microporous filter membrane and an OnGuard Ⅱ RP column; thus, the pretreatment steps are simple. The eight organic amines showed a good linear relationship within a certain concentration range, and the coefficient of determinations (R²) were greater than 0.998. The limits of detection (LODs) and quantification (LOQs) were determined from the mass concentrations of the organic amines corresponding to signal-to-noise ratios (S/N) of 3 and 10, respectively. LODs of 0.02-0.08 mg/L and LOQs of 0.07-0.27 mg/L were determined from a 1.0 μL sample injection. The actual recoveries ranged from 93.0% to 111%, and the relative standard deviations (RSDs, n=5) ranged from 0.31% to 1.2%. The results indicated that the proposed method has good accuracy and precision; thus, it is suitable for the determination of various organic amines in desulfurization solution.

Key words: ion chromatography (IC), organic amines, desulfurization solution

CLC Number:

O658

GAO Lihong, JIANG Zhenbang, ZHENG Hongguo, LI Wenhui. Simultaneous determination of eight organic amines in desulfurization solution by ion chromatography[J]. Chinese Journal of Chromatography, 2024, 42(5): 452-457.

Figures/Tables 6

References

[1]	Liu H. China Energy and Environmental Protection, 2019, 41(3): 122
[1]	刘恒. 能源与环保, 2019, 41(3): 122
[2]	Li L T, Peng Z L, Zhang Y H, et al. Petrochemical Technology & Application, 2019, 37(6): 417
[2]	李兰婷, 彭振磊, 张育红, 等. 石化技术与应用, 2019, 37(6): 417
[3]	Li L T, Peng Z L, Zhang Y H, et al. Petrochemical Technology, 2020, 49(1): 93
[3]	李兰婷, 彭振磊, 张育红, 等. 石油化工, 2020, 49(1): 93
[4]	Chen X, Zhang G W. Journal of Nanchang University (Natural Science), 2014, 38(2): 143
[4]	陈希, 张国文. 南昌大学学报(理科版), 2014, 38(2): 143
[5]	Wang X, Sun Y Y, Zhang Q L. Environmental Protection of Chemical Industry, 2023, 43(4): 556
[5]	王雪, 孙阳洋, 章巧林. 化工环保, 2023, 43(4): 556
[6]	Xu G L, Xu H. Chemical Production and Technology, 2011, 18(4): 53
[6]	徐国良, 徐辉. 化工生产与技术, 2011, 18(4): 53
[7]	Chen M S, Liang Z, Li X J, et al. Fujian Analysis & Testing, 2017, 26(3): 1
[7]	陈旻实, 梁震, 李小晶, 等. 福建分析测试, 2017, 26(3): 1
[8]	Zhao S, Yang Y Q, Li X T, et al. Chinese Journal of Analysis Laboratory, 2016, 35(12): 1383
[8]	赵申, 杨一青, 李晓韬, 等. 分析试验室, 2016, 35(12): 1383
[9]	Song W D, Xu M L, Gao Y H, et al. Chinese Journal of Analysis Laboratory, 2020, 39(5): 590
[9]	宋卫得, 许美玲, 高尧华, 等. 分析试验室, 2020, 39(5): 590
[10]	Peng X L, Jiang Z B, Li R Y. Chemical Analysis and Meterage, 2014, 23(Z1): 52
[10]	彭绪玲, 姜振邦, 李仁勇. 化学分析计量, 2014, 23(Z1): 52
[11]	Yu B B, Yan Z C, Cheng X Y, et al. Environmental Science and Technology, 2021, 34(4): 50
[11]	余彬彬, 严朝朝, 成晓叶, 等. 环境科技, 2021, 34(4): 50
[12]	Zhang Y Q, Lu W Y, Wang X Q, et al. Environmental Monitoring Management and Technology, 2020, 32(4): 48
[12]	张嫣秋, 陆伟英, 王嬉巧, 等. 环境监测管理与技术, 2020, 32(4): 48
[13]	Luo Q Q, Huo S X. Chemical Analysis and Meterage, 2022, 31(3): 48
[13]	罗全迁, 霍世欣. 化学分析计量, 2022, 31(3): 48
[14]	Chen M S, Liang Z, Tang H Y, et al. Chinese Journal of Analysis Laboratory, 2017, 26(3): 1
[14]	陈旻实, 梁震, 唐寰宇, 等. 分析试验室, 2017, 26(3): 1
[15]	Liu Z Y, Wang X F, Li M, et al. Journal of Earth Environment, 2023, 14(2): 229
[15]	刘智艺, 王新锋, 李敏, 等. 地球环境学报, 2023, 14(2): 229
[16]	Tang Z K, Wan H H, Li H, et al. Chinese Journal of Chromatography, 2023, 41(9): 799
[16]	唐泽坤, 万慧慧, 李红, 等. 色谱, 2023, 41(9): 799
[17]	Lai J J, Chen M S, Tang X, et al. China Port Science and Technology, 2021(4): 68
[17]	赖佳佳, 陈旻实, 唐熙, 等. 中国口岸科学技术, 2021(4): 68
[18]	Zou Y C, Li W F, Liu L Y. Physical Testing and Chemical Analysis (Part B: Chemical Analysis), 2022, 58(7): 836
[18]	邹阅超, 李伟芳, 刘绿叶. 理化检验(化学分册), 2022, 58(7): 836
[19]	Liu F X, Bi X H, Ren Z F, et al. Chinese Journal of Analytical Chemistry, 2017, 45(4): 477
[19]	刘凤娴, 毕新慧, 任照芳, 等. 分析化学, 2017, 45(4): 477
[20]	Xiao W, Ma H Q, Hao X H. Chemical Analysis and Meterage, 2023, 32(8): 30
[20]	肖湾, 马红青, 郝晓红. 化学分析计量, 2023, 32(8): 30

Compound	Linear range/(mg/L)	R²	Linear equation	LOD/(mg/L)	LOQ/(mg/L)
MEA	10-200	0.9993	y=0.0071x-0.0011	0.05	0.17
AMP	10-200	0.9999	y=0.0044x-0.0137	0.08	0.27
MDEA	10-200	0.9994	y=0.0023x+0.0065	0.05	0.17
DEEA	10-200	0.9999	y=0.0036x-0.0060	0.04	0.14
AEEA	10-200	0.9980	y=0.0036x+0.0164	0.02	0.07
PZ	10-200	0.9990	y=0.0046x+0.0102	0.02	0.07
HEPZ	10-200	0.9992	y=0.0046x+0.0357	0.03	0.10
DETA	10-200	0.9988	y=0.0068x+0.0512	0.04	0.14

Compound	Linear range/(mg/L)	R²	Linear equation	LOD/(mg/L)	LOQ/(mg/L)
MEA	10-200	0.9993	y=0.0071x-0.0011	0.05	0.17
AMP	10-200	0.9999	y=0.0044x-0.0137	0.08	0.27
MDEA	10-200	0.9994	y=0.0023x+0.0065	0.05	0.17
DEEA	10-200	0.9999	y=0.0036x-0.0060	0.04	0.14
AEEA	10-200	0.9980	y=0.0036x+0.0164	0.02	0.07
PZ	10-200	0.9990	y=0.0046x+0.0102	0.02	0.07
HEPZ	10-200	0.9992	y=0.0046x+0.0357	0.03	0.10
DETA	10-200	0.9988	y=0.0068x+0.0512	0.04	0.14

Compound	Background/ (g/L)	Added/ (g/L)	Found/ (g/L)	Recovery/ %	RSD/ %	Compound	Background/ (g/L)	Added/ (g/L)	Found/ (g/L)	Recovery/ %	RSD/ %
MEA	8.45	5.0	13.4	99.0	0.51	AEEA	nd	1.0	1.10	110	0.87
		7.5	15.7	96.7	0.97			5.0	5.27	105	0.47
		16	24.0	97.2	0.85			20	20.5	103	0.88
AMP	nd	1.0	0.97	97.0	0.93	PZ	nd	1.0	0.98	98.0	0.93
		5.0	5.29	105	0.46			5.0	5.23	104	0.43
		20	19.2	96.0	1.2			20	19.8	99.0	0.98
MDEA	10.1	5.0	15.0	98.0	0.40	HEPZ	6.10	2.5	8.68	103	0.31
		10	19.6	95.0	0.78			5.0	11.2	102	0.34
		20	29.3	96.0	0.95			12	17.9	98.3	0.63
DEEA	nd	1.0	0.93	93.0	0.75	DETA	nd	1.0	1.07	107	0.84
		5.0	5.01	100	0.52			5.0	5.57	111	0.47
		20	19.6	98.0	1.0			20	20.3	102	0.68

Compound	Background/ (g/L)	Added/ (g/L)	Found/ (g/L)	Recovery/ %	RSD/ %	Compound	Background/ (g/L)	Added/ (g/L)	Found/ (g/L)	Recovery/ %	RSD/ %
MEA	8.45	5.0	13.4	99.0	0.51	AEEA	nd	1.0	1.10	110	0.87
		7.5	15.7	96.7	0.97			5.0	5.27	105	0.47
		16	24.0	97.2	0.85			20	20.5	103	0.88
AMP	nd	1.0	0.97	97.0	0.93	PZ	nd	1.0	0.98	98.0	0.93
		5.0	5.29	105	0.46			5.0	5.23	104	0.43
		20	19.2	96.0	1.2			20	19.8	99.0	0.98
MDEA	10.1	5.0	15.0	98.0	0.40	HEPZ	6.10	2.5	8.68	103	0.31
		10	19.6	95.0	0.78			5.0	11.2	102	0.34
		20	29.3	96.0	0.95			12	17.9	98.3	0.63
DEEA	nd	1.0	0.93	93.0	0.75	DETA	nd	1.0	1.07	107	0.84
		5.0	5.01	100	0.52			5.0	5.57	111	0.47
		20	19.6	98.0	1.0			20	20.3	102	0.68

No.	MEA	AMP	MDEA	DEEA	AEEA	PZ	HEPZ	DETA
1	101	<LOD	168	<LOD	<LOD	<LOD	56.5	<LOD
2	85.3	<LOD	140	<LOD	<LOD	<LOD	38.8	<LOD
3	82.0	<LOD	131	<LOD	<LOD	<LOD	33.2	<LOD
4	8.45	<LOD	10.1	<LOD	<LOD	<LOD	6.10	<LOD