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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
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1.西南科技大学材料科学与工程学院;2.西安近代化学研究所

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国防科工局技术基础科研项目 JSJL2014208A006;西南科技大学研究生创新基金资助 17ycx019国防科工局技术基础科研项目(JSJL2014208A006);西南科技大学研究生创新基金资助(17ycx019)


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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    摘要:

    为了测定含能增塑剂二缩三乙二醇二硝酸酯(TEGDN)中的阴离子杂质,采用制备液相色谱-离子色谱法对TEGDN中的阴离子进行定性定量分析。考察了制备液相色谱实验中不同流动相比例、进样量、收集时间对TEGDN中杂质阴离子的分离和收集效果的影响以及离子色谱实验中淋洗液体系和淋洗液流速对阴离子分离效果的影响。结果表明,优化后的制备液相色谱条件为:Eclipse XDB-C18色谱柱(250 mm×9.4 mm,5.0 μm),流动相V甲醇∶V=50∶50,流速1.5 mL·min-1,检测波长210 nm,柱温30 ℃,进样体积0.25 mL;优化后的离子色谱条件为:Metrosep A Supp 5型阴离子分析柱(250 mm×4.0 mm,5.0 μm),淋洗液Na2CO3(3.2 mmol·L-1)/NaHCO3(1.0 mmol·L-1),流速0.7 mL·min-1,抑制型电导检测器,柱温40 ℃,进样体积20 μL。在优化的制备色谱条件下,TEGDN中的杂质阴离子得到有效分离和收集,在离子色谱测定中,各阴离子线性关系良好,相关系数均大于0.999,检出限为0.0025~0.0100 μg·mL-1,精密度和重复性试验(n=6)的相对标准偏差均小于2.0%,平均加标回收率为95.5%~103.5%。该方法灵敏度高,重现性好,可用于测定TEGDN7中的阴离子杂质。

    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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引用本文

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. DOI:10.11943/CJEM2018165.
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. DOI:10.11943/CJEM2018165.

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历史
  • 收稿日期: 2018-06-24
  • 最后修改日期: 2019-02-28
  • 录用日期: 2018-11-07
  • 在线发布日期: 2019-02-24
  • 出版日期: 2019-06-25