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Citation: LI Dan-Ni, LIU Wen-Wen, LIAN Hong-Zhen, ZHU Jin-Song. Quality Control Method for Tris (2,4-di-tert-butylphenyl) phosphite Production and Identification of Its Impurities[J]. Chinese Journal of Applied Chemistry, ;2005, 22(5): 511-516. shu

Quality Control Method for Tris (2,4-di-tert-butylphenyl) phosphite Production and Identification of Its Impurities

1.
a Key Laboratory of Analytical Chemistry for Life Science, The Ministry of Education, Center of Materials Analysis, Department of Chemistry, Nanjing University, Nanjing 210093;
2.
b Nanjing YPC Fine Chemical Industry Company Ltd., Nanjing

Corresponding author: LIAN Hong-Zhen,
Received Date: 26 July 2004
Available Online: 26 December 2004
Fund Project: 南京大学分析测试基金资助项目(04CA5) (04CA5)

This paper presents a high-performance liquid chromatography-UV detection analytical method for the determination of tris (2,4-di-tert-butylphenyl) phosphite (TBP) and its poisonous impurity 2,4-di-tert-butylphenol (DBP).The separation between TBP and DBP was performed on a Kromasil C₁₈ column,5 μm,150 mm×4.6 mm (i.d.),and the quantitation was achieved with UV detection at 275 nm.The column temperature was maintained at 30℃.The mobile phase was a mixture of methanol and water and run at a flow rate of 1.0 mL/min,and a two-step linear gradient elution,0~5 min,V(methanol):V(water)=95:5;5~25 min,V(methanol):V(water)=100:0,was adopted.The calibration curves were linear in the concentration ranges of 1.0×10^-6~1.0×10^-3 g/mL of TBP and 1.0×10^-7~1.0×10^-4 g/mL of DBP,respec-tively,with correlation coefficients of 0.999 94 and 0.999 95.The detection limits were 1.0×10^-7 g/mL for TBP and 1.0×10^-8 g/mL for DBP.Good reproducibility was obtained for the determinations of TBP and DBP in real industrial samples with relative standard deviations of 0.1% and 1.8%,respectively.The DBP analysis result obtained by HPLC were compared with that by spectrophotometry,and it was found that the spectrometric method was unable to determine DBP in TBP accurately.Two impurities were identified by LC-MS.The structure of another impurity was estimated according to its UV-Vis spectrum and chromatographic behavior.All these three impurities in antioxidant 168 were TBP derivatives with fewer tert-butyl substituents.When an isocratic elution was used:(0~20 min,V(methanol):V(water)=100:0),this method was applied to analyze TBP in composite antioxidants with a relative standard deviation of 0.7% and a recovery rate of 101%.
- tris(di-tert-butylphenyl)phosphite,
- di-tert-butylphenol,
- LC-MS,
- HPLC,
- UV-Vis spectrum
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