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<p>Accurate determination of trace anions in electronic-grade N-methylpyrrolidone (NMP) is crucial for ensuring the reliability of lithium-ion batteries and semiconductor devices. However, severe interference from the massive organic matrix prevents conventional one-dimensional ion chromatography (1D-IC) from meeting the stringent requirements of sub-microgram-per-kilogram (µg/kg) level detection. To address this challenge, an automated, online two-dimensional ion exclusion–ion exchange chromatography (2D-ICE-IC) method integrated with a valve-switching technique was developed. By introducing ion exclusion chromatography (ICE) in the first dimension, the complex NMP matrix and potential interfering components were eliminated, leveraging the distinctly different retention behaviors between the target anions and the organic background. Combined with large-volume injection and a precisely timed valve-switching program, the heart-cut target anions were captured on a concentrator column and subsequently transferred to the second-dimensional ion exchange system for high-sensitivity analysis. Under optimized conditions, five target anions (Cl⁻, Br⁻, NO₃⁻, SO₄²⁻, and PO₄³⁻) exhibited excellent linearity within the range of 0.5–20&#xa0;µg/kg (<i>r</i> &gt; 0.999), with limits of detection (LODs) as low as 0.006–0.021&#xa0;µg/kg. Spiked recoveries at low, medium, and high concentration levels ranged stably between 75% and 115%, with precisions (RSD, <i>n</i> = 6) below 5%. Operated within a Class 1000 cleanroom, this method effectively prevents secondary contamination and analyte loss typically associated with traditional offline sample pretreatment. Its high automation and exceptional selectivity offer a reliable and industry-applicable strategy for the purity control and quality assessment of high-purity, highly polar organic solvents.</p>

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Determination of Trace Anions in Electronic-Grade N-Methylpyrrolidone Using Two-Dimensional Ion Exclusion–Ion Exchange Chromatography Combined with a Valve-Switching Technique

  • 期刊论文

  • 发表日期：

    2026年8月3日

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  • Zhou Zheng,
  • Yan Lu,
  • Tao Ye,
  • Mijia Feng,
  • Songli Shen,
  • Dan Hu,
  • Xiaojie Xu,
  • Xin Shen

摘要

Accurate determination of trace anions in electronic-grade N-methylpyrrolidone (NMP) is crucial for ensuring the reliability of lithium-ion batteries and semiconductor devices. However, severe interference from the massive organic matrix prevents conventional one-dimensional ion chromatography (1D-IC) from meeting the stringent requirements of sub-microgram-per-kilogram (µg/kg) level detection. To address this challenge, an automated, online two-dimensional ion exclusion–ion exchange chromatography (2D-ICE-IC) method integrated with a valve-switching technique was developed. By introducing ion exclusion chromatography (ICE) in the first dimension, the complex NMP matrix and potential interfering components were eliminated, leveraging the distinctly different retention behaviors between the target anions and the organic background. Combined with large-volume injection and a precisely timed valve-switching program, the heart-cut target anions were captured on a concentrator column and subsequently transferred to the second-dimensional ion exchange system for high-sensitivity analysis. Under optimized conditions, five target anions (Cl⁻, Br⁻, NO₃⁻, SO₄²⁻, and PO₄³⁻) exhibited excellent linearity within the range of 0.5–20 µg/kg (r > 0.999), with limits of detection (LODs) as low as 0.006–0.021 µg/kg. Spiked recoveries at low, medium, and high concentration levels ranged stably between 75% and 115%, with precisions (RSD, n = 6) below 5%. Operated within a Class 1000 cleanroom, this method effectively prevents secondary contamination and analyte loss typically associated with traditional offline sample pretreatment. Its high automation and exceptional selectivity offer a reliable and industry-applicable strategy for the purity control and quality assessment of high-purity, highly polar organic solvents.