Citation: ZENG Kun, MA Yuan-Yuan, GUO Qing-Zhong, DUAN Tai-Cheng. Determination of Thionyl Chloride Residue in Terephthaloyl Chloride by Inductively Coupled Plasma-Optical Emission Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2019, 47(3): 410-414. doi: 10.19756/j.issn.0253-3820.181691 shu

Determination of Thionyl Chloride Residue in Terephthaloyl Chloride by Inductively Coupled Plasma-Optical Emission Spectrometry

1.
Materials Science and Engineering, Wuhan Institute of Technology, Wuhan 430074, China;
2.
Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022, China

Received Date: 31 October 2018
Revised Date: 26 December 2018

Fund Project: This work was supported by the National Natural Science Foundation of China (No. 21275138).

A method for determination of thionyl chloride(SOCl₂) residue in terephthaloyl chloride by inductively coupled plasma-optical emission spectrometry(ICP-OES) was developed. The samples were firstly dissolved with organic solvents and then subjected to liquid-liquid extraction, by which the hydrolization of thionyl chloride could lead to the formation of inorganic sulfate, which was then accurately determined by ICP-OES and the content of thionyl chloride residue thus could be calculated. The type of the organic solvent and its volume to sample mass ratio were optimized, and it was found that the sample could be readily dissolved in carbon tetrachloride as the solvent and the ratio of solvent volume to sample mass being 10 (mL:g). Also, the conditions for the extraction procedure were studied, and it was found that when the aqueous phase solution contained 10% (V/V) nitric acid and 2% (V/V) hydrogen peroxide and the shaking time was kept in about 2 min, the full hydrolization of thionyl chloride and the complete oxidation of H₂SO₃ could be accomplished, as well as a quick separation of the two organic/water phase was realized. The results showed that the limit of detection (LOD, 3s) of the method was 0.22 mg/kg (calculated as S), the relative standard deviation (RSD) was 2.1% for six real sample analysis, and the recoveries of spiked test were 92.7%-104.6%. The established method was finally applied to the analysis of the real samples collected from the purification process of the terephthaloyl chloride production plant and the results were highly in accordance with theoretically predicted value.
- Thionyl chloride,
- Terephthaloyl chloride,
- Inductively coupled plasma-optical emission spectrometry,
- Liquid-liquid extraction
1. [1]
2. [2]
3. [3]
4. [4]
5. [5]
6. [6]
7. [7]
8. [8]
9. [9]
10. [10]
11. [11]
12. [12]
13. [13]
14. [14]
15. [15]
16. [16]
17. [17]
18. [18]
1. [1]
  Yingran Liang , Fei Wang , Jiabao Sun , Hongtao Zheng , Zhenli Zhu . Construction and Application of a New Experimental Device for Determination of Alkaline Metal Elements by Plasma Atomic Emission Spectrometry Based on Solution Cathode Glow Discharge: An Alternative Approach for Fundamental Teaching Experiments in Emission Spectroscopy. University Chemistry, 2024, 39(5): 380-387. doi: 10.3866/PKU.DXHX202312024
2. [2]
  Jiandong Liu , Xin Li , Daxiong Wu , Huaping Wang , Junda Huang , Jianmin Ma . Anion-Acceptor Electrolyte Additive Strategy for Optimizing Electrolyte Solvation Characteristics and Electrode Electrolyte Interphases for Li||NCM811 Battery. Acta Physico-Chimica Sinica, 2024, 40(6): 2306039-0. doi: 10.3866/PKU.WHXB202306039
3. [3]
  Feiya Cao , Qixin Wang , Pu Li , Zhirong Xing , Ziyu Song , Heng Zhang , Zhibin Zhou , Wenfang Feng . Magnesium-Ion Conducting Electrolyte Based on Grignard Reaction: Synthesis and Properties. University Chemistry, 2024, 39(3): 359-368. doi: 10.3866/PKU.DXHX202308094
4. [4]
  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
5. [5]
  Liuyun Chen , Wenju Wang , Tairong Lu , Xuan Luo , Xinling Xie , Kelin Huang , Shanli Qin , Tongming Su , Zuzeng Qin , Hongbing Ji . Soft template-induced deep pore structure of Cu/Al₂O₃ for promoting plasma-catalyzed CO₂ hydrogenation to DME. Acta Physico-Chimica Sinica, 2025, 41(6): 100054-0. doi: 10.1016/j.actphy.2025.100054
6. [6]
  Xiting Zhou , Zhipeng Han , Xinlei Zhang , Shixuan Zhu , Cheng Che , Liang Xu , Zhenyu Sun , Leiduan Hao , Zhiyu Yang . Dual Modulation via Ag-Doped CuO Catalyst and Iodide-Containing Electrolyte for Enhanced Electrocatalytic CO₂ Reduction to Multi-Carbon Products: A Comprehensive Chemistry Experiment. University Chemistry, 2025, 40(7): 336-344. doi: 10.12461/PKU.DXHX202412070
7. [7]
  Qianli Ma , Tianbing Song , Tianle He , Xirong Zhang , Huanming Xiong . Sulfur-doped carbon dots: a novel bifunctional electrolyte additive for high-performance aqueous zinc-ion batteries. Acta Physico-Chimica Sinica, 2025, 41(9): 100106-0. doi: 10.1016/j.actphy.2025.100106
8. [8]
  Yajie Li , Bin Chen , Yiping Wang , Hui Xing , Wei Zhao , Geng Zhang , Siqi Shi . Inhibiting Dendrite Growth by Customizing Electrolyte or Separator to Achieve Anisotropic Lithium-Ion Transport: A Phase-Field Study. Acta Physico-Chimica Sinica, 2024, 40(3): 2305053-0. doi: 10.3866/PKU.WHXB202305053
9. [9]
  Aoyu Huang , Jun Xu , Yu Huang , Gui Chu , Mao Wang , Lili Wang , Yongqi Sun , Zhen Jiang , Xiaobo Zhu . Tailoring Electrode-Electrolyte Interfaces via a Simple Slurry Additive for Stable High-Voltage Lithium-Ion Batteries. Acta Physico-Chimica Sinica, 2025, 41(4): 100037-0. doi: 10.3866/PKU.WHXB202408007
10. [10]
  Yutong Dong , Huiling Xu , Yucheng Zhao , Zexin Zhang , Ying Wang . The Hidden World of Surface Tension and Droplets. University Chemistry, 2024, 39(6): 357-365. doi: 10.3866/PKU.DXHX202312022
11. [11]
  Yujing Chen , Hongqun Ouyang , Dan Zhao , Yanyan Chu , Zhengping Qiao . Recommendations for the Content and Instruction of the Physical Chemistry Experiment “Construction of Ternary Liquid-Liquid Phase Diagrams”. University Chemistry, 2025, 40(7): 359-366. doi: 10.12461/PKU.DXHX202409120
12. [12]
  Jianding LI , Junyang FENG , Huimin REN , Gang LI . Proton conductive properties of a Hf(Ⅳ)-based metal-organic framework built by 2,5-dibromophenyl-4,6-dicarboxylic acid. Chinese Journal of Inorganic Chemistry, 2025, 41(6): 1094-1100. doi: 10.11862/CJIC.20240464
13. [13]
  Chunai Dai , Yongsheng Han , Luting Yan , Zhen Li , Yingze Cao . Ideological and Political Design of Solid-liquid Contact Angle Measurement Experiment. University Chemistry, 2024, 39(2): 28-33. doi: 10.3866/PKU.DXHX202306065
14. [14]
  Hao Chen , Dongyue Yang , Gang Huang , Xinbo Zhang . Progress on Liquid Organic Electrolytes of Li-O₂ Batteries. Acta Physico-Chimica Sinica, 2024, 40(7): 2305059-0. doi: 10.3866/PKU.WHXB202305059
15. [15]
  Shiyi Chen , Jialong Fu , Jianping Qiu , Guoju Chang , Shiyou Hao . Waste medical mask-derived carbon quantum dots enhance the photocatalytic degradation of polyethylene terephthalate (PET) over BiOBr/g-C₃N₄ S-scheme heterojunction. Acta Physico-Chimica Sinica, 2026, 42(1): 100135-0. doi: 10.1016/j.actphy.2025.100135
16. [16]
  Linbao Zhang , Weisi Guo , Shuwen Wang , Ran Song , Ming Li . Electrochemical Oxidation of Sulfides to Sulfoxides. University Chemistry, 2024, 39(11): 204-209. doi: 10.3866/PKU.DXHX202401009
17. [17]
  Wei Peng , Baoying Wen , Huamin Li , Yiru Wang , Jianfeng Li . Exploration and Practice on Raman Scattering Spectroscopy Experimental Teaching. University Chemistry, 2024, 39(8): 230-240. doi: 10.3866/PKU.DXHX202312062
18. [18]
  Jiahe LIU , Gan TANG , Kai CHEN , Mingda ZHANG . Effect of low-temperature electrolyte additives on low-temperature performance of lithium cobaltate batteries. Chinese Journal of Inorganic Chemistry, 2025, 41(4): 719-728. doi: 10.11862/CJIC.20250023
19. [19]
  Zhuo Han , Danfeng Zhang , Haixian Wang , Guorui Zheng , Ming Liu , Yanbing He . Research Progress and Prospect on Electrolyte Additives for Interface Reconstruction of Long-Life Ni-Rich Lithium Batteries. Acta Physico-Chimica Sinica, 2024, 40(9): 2307034-0. doi: 10.3866/PKU.WHXB202307034
20. [20]
  Rui Yang , Hui Li , Qingfei Meng , Wenjie Li , Jiliang Wu , Yongjin Fang , Chi Huang , Yuliang Cao . Influence of PC-based Electrolyte on High-Rate Performance in Li/CrO_x Primary Battery. Acta Physico-Chimica Sinica, 2024, 40(9): 2308053-0. doi: 10.3866/PKU.WHXB202308053

Get Citation

PDF

XML

Metrics

PDF Downloads(13)
Abstract views(1129)
HTML views(147)

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