Citation: LIU Junyan, TIAN Wenqing, LI Jiwen, WANG Chuan, GU Songyuan. Determination of oxygenates in syngas-to-olefin products by solid phase extraction combined with gas chromatography-mass spectrometry[J]. Chinese Journal of Chromatography, ;2014, 32(11): 1280-1285. doi: 10.3724/SP.J.1123.2014.06043 shu

Determination of oxygenates in syngas-to-olefin products by solid phase extraction combined with gas chromatography-mass spectrometry

1.
Characterization & Analysis Department, Sinopec Shanghai Research Institute of Petrochemical Technology, Shanghai 201208, China

Corresponding author: LIU Junyan,
Received Date: 28 June 2014
Available Online: 14 August 2014

The syngas-to-olefin (SGTO) products mainly consist of hydrocarbons along with small amounts of oxygenates as the byproducts. A C18 solid-phase extraction (SPE) column was used for oxygenates enrichment in SGTO products. As the hydrophobic compounds, the hydrocarbons had stronger interaction with a C18 SPE column than oxygenates. Under the optimized elution conditions, the oxygenates were first eluted from the C18 SPE column with 60% (v/v) methanol solution. The fraction of oxygenates was then analyzed with gas chromatography-mass spectrometry (GC-MS) for qualification and gas chromatography-hydrogen flame ionization detection (GC-FID) for quantification. The FID response factors of n-alkanol and n-ketone were used for alkanols and ketones quantitative calculation and the method recoveries were 88%-98% and 64%-87% respectively. In the range of 197-4785 mg/L, good linear relationships of the FID responses with the corresponding mass concentrations of the standard samples were obtained with the linear regression coefficients greater than 0.99. Sixty-seven oxygenates were analyzed qualitatively and quantitatively. The results showed that the fraction of the oxygenates mainly consists of alkanols and ketones. The total content of the oxygenates in SGTO products was 6.2%. The enrichment method only requires a very small amount of sample and the total process can be completed within 10 min. The analysis results of SGTO product studies can provide the necessary basic data for SGTO catalysts and dynamics studies.
- solid-phase extraction (SPE),
- gas chromatography (GC),
- mass spectrometry (MS),
- hydrogen flame ionization detection (FID),
- oxygenate,
- syngas-to-olefin
1. [1]
  [1] Yang H J. Shandong Industrial Technology (杨海军. 山东工业技术), 2013(15): 122
2. [2]
  [2] Hu X T, Li Z Y, Huang G X. Petrochemical Technology (胡徐腾, 李振宇, 黄格省. 石油化工), 2012, 41(8): 869
3. [3]
  [3] Jiao Z K, Zhu L X, Sun J C, et al. Industrial Catalysis (焦祖凯, 朱连勋, 孙锦昌, 等. 工业催化), 2013, 21(7): 10
4. [4]
  [4] Zhang L P, Xin Z. Applied Chemical Industry (张丽平, 辛忠. 应用化工), 2009, 38(5): 731
5. [5]
  [5] Dong L, Yang X P. Petrochemical Technology (董丽, 杨学萍. 石油化工), 2012, 41(10): 1201
6. [6]
  [6] Huff Jr G A, Satterfleld C N, Wolf M H. Ind Eng Chem Fundam, 1983, 22(2): 258
7. [7]
  [7] Snavely K, Subramaniam B. Ind Eng Chem Res, 1997, 36: 4413
8. [8]
  [8] Dictor R A, Bell A T. Ind Eng Chem Fundam, 1984, 23: 252
9. [9]
  [9] Fan G X, Xu Y Y, Li Y, et al. Chinese Journal of Chromatography (樊改仙, 徐元源, 李莹, 等. 色谱), 2007, 25(6): 893
10. [10]
  [10] Ma N, Chen L, Xiong F. Shanghai Environmental Sciences (马娜, 陈玲, 熊飞. 上海环境科学), 2002, 21(3): 181
11. [11]
  [11] Wu M, Liu Z L, Tian S B, et al. Petroleum Processing and Petrochemicals (吴梅, 刘泽龙, 田松柏, 等. 石油炼制与化工), 2006, 37(7): 58
12. [12]
  [12] Ye C P, Feng J, Li W Y, et al. Journal of Taiyuan University of Technology (叶翠平, 冯杰, 李文英, 等. 太原理工大学学报), 2010, 41(5): 661
13. [13]
  [13] Zhou R, Sha X, Zhao G H, et al. Analytical Instrumentation (周蓉, 沙雪, 赵国辉, 等. 分析仪器), 2012(3): 95
14. [14]
  [14] Zhao H X, Liu H P, Yan Z Y. Chinese Journal of Chromatography (赵海香, 刘海萍, 闫早婴. 色谱), 2014, 32(3): 294
15. [15]
  [15] Jia Y Y, Tan J H, Xu C, et al. Chinese Journal of Chromatography (贾妍艳, 谭建华, 徐晨, 等. 色谱), 2014, 32(3): 263
16. [16]
  [16] Xu Y Q, Zhu X Y, Liu Z L, et al. Acta Petrolei Sinica: Petroleum Processing Section (徐延勤, 祝馨怡, 刘泽龙, 等. 石油学报: 石油加工), 2010, 26(3): 431
17. [17]
  [17] Luo F, Fei X Q, Fang X Z, et al. Journal of Instrumental Analysis (罗凡, 费学谦, 方学智, 等. 分析测试学报), 2011, 30(6): 696
1. [1]
  Siwei Hou , Yaxin Niu , Guanglu Zhang , Yanmei Yang , Xu Wang , Zhenzhen Chen . Application of Solid-Phase Microextraction and Mass Spectrometry in Environmental Detection. University Chemistry, 2026, 41(3): 297-306. doi: 10.12461/PKU.DXHX202504078
2. [2]
  Shunü Peng , Huamin Li , Zhaobin Chen , Yiru Wang . Simultaneous Application of Multiple Quantitative Analysis Methods in Gas Chromatography for the Determination of Active Ingredients in Traditional Chinese Medicine Preparations. University Chemistry, 2025, 40(10): 243-249. doi: 10.12461/PKU.DXHX202412043
3. [3]
  Zelin Wang , Gang Liu , Mengran Wang , Peiyu Zhang , Aixin Song , Jingcheng Hao , Jiwei Cui . Application of Instrumental Analysis in the Detection of Organic Components in Liquor. University Chemistry, 2025, 40(11): 318-326. doi: 10.12461/PKU.DXHX202502077
4. [4]
  Jingming Li , Bowen Ding , Nan Li , Nurgul . Application of Comparative Teaching Method in Experimental Project Design of Instrumental Analysis Course: A Case Study in Chromatography Experiment Teaching. University Chemistry, 2024, 39(8): 263-269. doi: 10.3866/PKU.DXHX202312078
5. [5]
  Wei Shao , Wanqun Zhang , Pingping Zhu , Wanqun Hu , Qiang Zhou , Weiwei Li , Kaiping Yang , Xisheng Wang . Design and Practice of Ideological and Political Cases in the Course of Instrument Analysis Experiment: Taking the GC-MS Experiment as an Example. University Chemistry, 2024, 39(2): 147-154. doi: 10.3866/PKU.DXHX202309048
6. [6]
  Zunxiang Zeng , Yuling Hu , Yufei Hu , Hua Xiao . Analysis of Plant Essential Oils by Supercritical CO₂Extraction with Gas Chromatography-Mass Spectrometry: An Instrumental Analysis Comprehensive Experiment Teaching Reform. University Chemistry, 2024, 39(3): 274-282. doi: 10.3866/PKU.DXHX202309069
7. [7]
  Yanhui Zhong , Ran Wang , Zian Lin . Analysis of Halogenated Quinone Compounds in Environmental Water by Dispersive Solid-Phase Extraction with Liquid Chromatography-Triple Quadrupole Mass Spectrometry. University Chemistry, 2024, 39(11): 296-303. doi: 10.12461/PKU.DXHX202402017
8. [8]
  Ke Qiu , Fengmei Wang , Mochou Liao , Kerun Zhu , Jiawei Chen , Wei Zhang , Yongyao Xia , Xiaoli Dong , Fei Wang . A Fumed SiO₂-based Composite Hydrogel Polymer Electrolyte for Near-Neutral Zinc-Air Batteries. Acta Physico-Chimica Sinica, 2024, 40(3): 2304036-0. doi: 10.3866/PKU.WHXB202304036
9. [9]
  Hao Wu , Zhen Liu , Dachang Bai . ¹H NMR Spectrum of Amide Compounds. University Chemistry, 2024, 39(3): 231-238. doi: 10.3866/PKU.DXHX202309020
10. [10]
  Mei-Xia Yang , Zhen-Hong He , Long-Rui Wang , You-Xing Yang . Route for Turning Waste CH₄ and CO₂ into Valuable Products: Reforming for Syngas. University Chemistry, 2026, 41(2): 197-207. doi: 10.12461/PKU.DXHX202503012
11. [11]
  Xiaowu Zhang , Pai Liu , Qishen Huang , Shufeng Pang , Zhiming Gao , Yunhong Zhang . Acid-Base Dissociation Equilibrium in Multiphase System: Effect of Gas. University Chemistry, 2024, 39(4): 387-394. doi: 10.3866/PKU.DXHX202310021
12. [12]
  Chongjing Liu , Yujian Xia , Pengjun Zhang , Shiqiang Wei , Dengfeng Cao , Beibei Sheng , Yongheng Chu , Shuangming Chen , Li Song , Xiaosong Liu . Understanding Solid-Gas and Solid-Liquid Interfaces through Near Ambient Pressure X-Ray Photoelectron Spectroscopy. Acta Physico-Chimica Sinica, 2025, 41(2): 100013-0. doi: 10.3866/PKU.WHXB202309036
13. [13]
  Jiao CHEN , Yi LI , Yi XIE , Dandan DIAO , Qiang XIAO . Vapor-phase transport of MFI nanosheets for the fabrication of ultrathin b-axis oriented zeolite membranes. Chinese Journal of Inorganic Chemistry, 2024, 40(3): 507-514. doi: 10.11862/CJIC.20230403
14. [14]
  Qi Zhang , Ziyu Liu , Hongxia Tan , Jun Tong , Dazhen Xu . Research Progress on Direct Synthesis of β-Hydroxy Sulfones via Difunctionalization of Olefins. University Chemistry, 2025, 40(11): 199-209. doi: 10.12461/PKU.DXHX202412064
15. [15]
  Yuanchun Pan , Xinyun Lin , Leyi Yang , Wenya Hu , Dekui Song , Nan Liu . Artificial Intelligence Science Practice: Preparation of Electronic Skin by Chemical Vapor Deposition of Graphene. University Chemistry, 2025, 40(11): 272-280. doi: 10.12461/PKU.DXHX202412052
16. [16]
  Zhuoming Liang , Ming Chen , Zhiwen Zheng , Kai Chen . Multidimensional Studies on Ketone-Enol Tautomerism of 1,3-Diketones By ¹H NMR. University Chemistry, 2024, 39(7): 361-367. doi: 10.3866/PKU.DXHX202311029
17. [17]
  Xiaofeng Zhu , Bingbing Xiao , Jiaxin Su , Shuai Wang , Qingran Zhang , Jun Wang . Transition Metal Oxides/Chalcogenides for Electrochemical Oxygen Reduction into Hydrogen Peroxides. Acta Physico-Chimica Sinica, 2024, 40(12): 2407005-0. doi: 10.3866/PKU.WHXB202407005
18. [18]
  Xiaotian ZHU , Fangding HUANG , Wenchang ZHU , Jianqing ZHAO . Layered oxide cathode for sodium-ion batteries: Surface and interface modification and suppressed gas generation effect. Chinese Journal of Inorganic Chemistry, 2025, 41(2): 254-266. doi: 10.11862/CJIC.20240260
19. [19]
  Mingyang Men , Jinghua Wu , Gaozhan Liu , Jing Zhang , Nini Zhang , Xiayin Yao . Sulfide Solid Electrolyte Synthesized by Liquid Phase Approach and Application in All-Solid-State Lithium Batteries. Acta Physico-Chimica Sinica, 2025, 41(1): 100004-0. doi: 10.3866/PKU.WHXB202309019
20. [20]
  Runjie Li , Hang Liu , Xisheng Wang , Wanqun Zhang , Wanqun Hu , Kaiping Yang , Qiang Zhou , Si Liu , Pingping Zhu , Wei Shao . 氨基酸的衍生及手性气相色谱分离创新实验. University Chemistry, 2025, 40(6): 286-295. doi: 10.12461/PKU.DXHX202407059

Get Citation

PDF

XML

Metrics

PDF Downloads(0)
Abstract views(445)
HTML views(23)

通讯作者: 陈斌, bchen63@163.com

1.
沈阳化工大学材料科学与工程学院沈阳 110142