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
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沈阳化工大学材料科学与工程学院沈阳 110142