首页|期刊导航|分析化学|基于脉冲高压消减电荷累积的四极杆质谱检测技术研究

基于脉冲高压消减电荷累积的四极杆质谱检测技术研究OA

Research on Quadrupole Mass Spectrometry Analysis Technology Based on Pulsed High Voltage Charge Accumulation Mitigation Method

中文摘要英文摘要

稳定性是质谱仪器的关键核心指标,直接影响实验结果的准确性和可靠性.然而,在四极杆固定陶瓷表面存在的电荷累积现象会使离子通过率和质谱峰形的半高峰宽(FWHM)发生变化,导致仪器稳定性衰减.为研究电荷累积现象对仪器稳定性的作用机理及影响程度,进行了仿真实验.结果表明,陶瓷带电会使四极场畸变,导致离子运动轨迹偏移;对陶瓷电极施加的电压越高,各质量段的质谱峰形变化越明显,对离子通过率和FWHM的影响越严重;当施加电压为20 V时,离子通过率减小53.3%,FWHM偏移0.23 amu.针对上述问题,提出了脉冲高压消减电荷累积方法.本方法不仅包括常规扫描的稳定过程和扫描过程,还包括脉冲高压电荷清空过程.在清空过程中,施加幅值约为500 V的直流高压和峰峰值约为6000 V的射频高压,实现陶瓷累积电荷的定时清除.为验证脉冲高压消减电荷累积方法的有效性,进行FWHM变化监测及3种化合物混和标样(六氯苯、六溴苯和十溴联苯醚)的稳定性对比实验.峰宽实验中,分别采用有无脉冲高压消减电荷累积方法对全氟三丁胺的碎片离子进行监测.结果表明,FWHM变化率由10%减小至4.4%,脉冲高压消减电荷累积方法可有效减小质谱峰形的FWHM变化.采用两种方法分别对3种化合物混合标样连续测试40次,峰面积的平均相对标准偏差由8.61%减小至3.93%,表明脉冲高压消减电荷累积方法对提高质谱仪器的稳定性有明显效果.

The stability of mass spectrometers is a key indicator,directly affecting the accuracy and reliability of experimental results.Nevertheless,charge accumulation on the fixed ceramic insulators of quadrupole alters the ion transmission efficiency and the full width at half maximum(FWHM)of mass spectral peaks,thus degrading instrument stability.To quantify the influence of charge accumulation on stability,simulation experiments were carried out.The simulation results revealed that charged ceramics caused obvious deflection of ion trajectories and distortion of the quadrupole field.Moreover,greater bias voltages applied to the ceramics led to more severe spectral peak variations.At a ceramic voltage of 20 V,the ion transmission efficiency decreased by 53.3%,the FWHM shifted by 0.23 amu,and the adverse effect intensified with the increase of mass-to-charge ratio.To solve this issue,the pulsed high voltage charge accumulation mitigation method was proposed.This method consisted of stabilization process,scanning process,and charge elimination process.In the elimination process,a DC high voltage of approximately 500 V amplitude and an RF high voltage with a peak-to-peak value of approximately 6000 V were applied to periodically eliminating charges.Two validation experiments,including FWHM drift monitoring and stability comparison of the mixed standard solution,were performed to verify the performance of the proposed method.In FWHM test,fragment ions of perfluorotributylamine were monitored under the conditions with and without the pulsed high voltage charge accumulation mitigation method.For the stability test,40 consecutive injections of a mixed solution containing hexachlorobenzene,hexabromobenzenen and decabromodiphenyl ether were tested with the two working modes.The average relative standard deviation of peak areas for the three analytes was reduced from 8.61%to 3.93%,which indicated that the proposed method remarkably improved the stability of the mass spectrometer.

孙澎勇;林一明;孟坚鑫;张敬;曹祥宽;沈林杰

杭州海康威视数字技术股份有限公司,杭州 310053杭州海康威视元物智科技有限公司,杭州 310053杭州海康威视数字技术股份有限公司,杭州 310053杭州海康威视数字技术股份有限公司,杭州 310053杭州海康威视元物智科技有限公司,杭州 310053杭州海康威视元物智科技有限公司,杭州 310053

质谱仪器稳定性电荷累积脉冲高压消减电荷累积方法质谱峰形

Mass spectrometer stabilityCharge accumulationPulse high voltage charge accumulation mitigation methodMass spectral peak profiles

《分析化学》 2026 (9)

1557-1564,中插21-中插22,10

杭州海康威视数字技术股份有限公司企业自主研发项目(No.PJ08PD20240115288)资助. Supported by the Independent R&D Project of Hangzhou Hikvision Digital Technology Co.,Ltd.(No.PJ08PD20240115288).

10.19756/j.issn.0253-3820.261165

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