色谱2025，Vol.43Issue(3)：237-244,8.DOI:10.3724/SP.J.1123.2024.04010
二维离子排斥-离子交换色谱配合阀切换技术测定G2级磷酸中的痕量阴离子
Determination of trace anions in G2-grade phosphoric acid using two-dimensional ion-exclusion-ion-exchange chromatography with valve-switching technology
摘要
Abstract
This study established a method for determining trace anions in G2-grade phosphoric acid under ultra-clean conditions that used two-dimensional ion-exclusion-ion-exchange chro-matography coupled with valve-switching technology.The optimal flow rate of ultrapure water through the ion-exclusion column in the first dimension was determined to be 0.5 mL/min through comparative experiments.The valve-switching window was optimized to minimize en-riching PO43-on the anion-enrichment column and reduce interference from the phosphoric-acid matrix.The use of external water mode for the suppressor led to lower baseline noise,and op-timizing the elution program of the second dimension enabled target trace anions to be well sep-arated,thereby avoiding the risk of a false positive for NO3-.The anions of Cl-,Br-,NO3-,and SO42-exhibited good linearities within the 0.5-20 μg/kg,with correlation coefficients≥0.999.The limits of detection(LODs)and quantification(LOQs)were 0.09-0.29 μg/kg and 0.29-0.97 μg/kg,respectively.The spiked recoveries of each anion at four spiked levels ranged from 91.7% to 103.6%,with RSDs of 0.1%-4.9% .The developed method demonstrated excellent stability through repeated injections,and low detection limits;it is highly precise and accurate,and meets the detection requirements for trace anions in G2-grade phosphoric acid.Additional-ly,retention-time comparisons with single standard substances led to the discovery of other phosphorus-related anions and anion clusters,such as hypophosphite(HPO3-)and hexameta-phosphate(PO3-)6,in G2-grade phosphoric acid,in addition to conventional anions.This find-ing is theoretically and practically significant for the future development of purification proces-ses for higher-purity phosphoric acid.关键词
电子级磷酸/痕量阴离子/阀切换/二维离子色谱Key words
electronic grade phosphoric acid/trace anions/valve switching/two-dimensional ion chromatography(2D-IC)分类
化学引用本文复制引用
王佳鼎,唐高,鹿燕,卢珩俊,叶涛..二维离子排斥-离子交换色谱配合阀切换技术测定G2级磷酸中的痕量阴离子[J].色谱,2025,43(3):237-244,8.基金项目
浙江省市场监管局"雏鹰计划"培育项目(CY2022005) （CY2022005）
浙江省教育厅科研资助项目(Y202353765).Zhejiang Provincial Market Supervision Bureau"Eagle Program"Cultivation Project(No.CY2022005) （Y202353765）
Zhe-jiang Provincial Department of Education Research Grant Program(No.Y202353765). （No.Y202353765）
