CHINESE JOURNAL OF ENERGETIC MATERIALS
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Determination of Anionic Impurities in Triethylene Glycol Dinitrate (TEGDN) by Preparative Liquid Chromatography-Ion Chromatography Method
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1.School of Materials Science and Engineering, Southwest University of Science and Technology, Mianyang 621010, China;2.Xi′an Modern Chemistry Research Institute, Xi''an 710065, China

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    Abstract:

    To determine anionic impurities in energetic plasticizer triethylene glycol dinitrate (TEGDN) , the anions in TEGDN were qualitatively and quantitatively analyzed by a preparative liquid chromatography-ion chromatography method. The effect of different mobile phase ratio, injection volume and collection time on the effect of separation and collection of anionic impurities in TEGDN in preparative liquid chromatographic experiments, and the effect of eluent system and eluent flow rate on the separation effect of anions in ion chromatographic experiments were investigated. Results show that the preparative liquid chromatographic conditions after optimization are: Eclipse XDB-C18 chromatographic column (250 mm×9.4 mm, 5.0 μm); mobile phase, Vmethanol∶Vwater=50∶50; flow rate, 1.5 mL·min-1; detection wavelength, 210 nm; column temperature, 30 ℃ ; injection volume, 0.25 mL. The ion chromatographic conditions after optimization are: Metrosep A Supp 5 anion analysis column (250 mm× 4.0 mm, 5.0 μm); 3.2 mmol·L-1 Na2CO3 / 1.0 mmol·L-1 NaHCO3 solution as eluent ; flow rate, 0.7 mL·min-1 ; suppression conductivity detector ; column temperature, 40 ℃ ; injection volume, 20 μL. Under the optimized preparative liquid chromatographic conditions, anionic impurities in TEGDN are effectively separated and collected. Under the optimized ion chromatographic conditions, the linearity of the anions is good, the linear correlation coefficients are greater than 0.999 ; the detection limits of anions are 0.0025-0.0100 μg·mL-1. The relative standard deviations of the precision test (n=6) and the repeatability test (n=6) are less than 2.0%, the average recoveries of anions are 95.5%-103.5%. The method has high sensitivity and good reproducibility, can be used for the determination of the anionic impurities in TEGDN.

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陈爽,康莹,胡银,等.制备液相色谱-离子色谱法测定二缩三乙二醇二硝酸酯(TEGDN)中阴离子杂质[J].含能材料,2019,27(6):516-520.
CHEN Shuang, KANG Ying, HU Yin, et al. Determination of Anionic Impurities in Triethylene Glycol Dinitrate (TEGDN) by Preparative Liquid Chromatography-Ion Chromatography Method[J]. Chinese Journal of Energetic Materials,2019,27(6):516-520.

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History
  • Received:June 24,2018
  • Revised:February 28,2019
  • Adopted:November 07,2018
  • Online: February 24,2019
  • Published: June 25,2019