Citation: HU Zhong-Yang, YE Ming-Li, WU Shu-Chao, PAN Guang-Wen, ZHANG Ting-Ting, LIU LÜ-Ye. Determination of Impurity Anions in High Pure Fluoride Reagents by Ion Chromatography with Column-Switching[J]. Chinese Journal of Analytical Chemistry, ;2012, 40(11): 1703-1708. doi: 10.3724/SP.J.1096.2012.20213 shu

Determination of Impurity Anions in High Pure Fluoride Reagents by Ion Chromatography with Column-Switching

1.
¹ Thermofisher Scientific Corporation, Shanghai 201203, China;

Corresponding author: HU Zhong-Yang,
Received Date: 2 March 2012
Available Online: 4 June 2012
Fund Project: 本文系浙江大学国家重点实验室开放基金项目(No. 2011KF07) (No. 2011KF07)安徽省教育厅高校科研项目(No. KJ2011B211)资助 (No. KJ2011B211)

A method was developed for the determination of trace anions (Cl^-, NO₃^-, PO₄^3- and SO₄^2-) in high pure fluoride reagents by ion chromatography (IC) with column-switching. Ion excluding column IonPac ICE-AS6 was used in the first step to separate the trace anion analytes from the high concentrated fluoride using deionized water as the mobile phase, separated analytes were enriched in the pre-concentration column IonPac TAC-ULP1 at the same time. By using a mixture of 4.5 mmol/L Na₂CO₃-0.8 mmol/L NaHCO₃ as the eluent at a flow rate of 1.2 mL/min, the analytes were eluted from the pre-concentrated column after switching the pre-concentrated column into the analytical system. The separation of the analytes was performed with IonPac AG23 (50 mm × 4 mm) as guard column and IonPac AS23 (250 mm×4 mm) as analytical column, and the detection was performed by suppressed conductivity detector. As a result, the linear ranges of the method for Cl^-, NO₃^-, PO₄^3- and SO₄^2- were 0.02-5.0 mg/L (r=0.9996), 0.02-5.0 mg/L (r=0.9999), 0.05-10.0 mg/L (r=0.9998), 0.02-5.0 mg/L (r=0.9997) respectively. The average recoveries were 92.0%-103.5% with the relative standard deviations (RSD, n=7) less than 3.0%. The detection limits (S/N=3) were 0.2, 0.6, 3.0 and 0.5 mg/kg for Cl^-, NO₃^-, PO₄^3-and SO₄^2-, respectively.
- Ion chromatography,
- Column switching,
- Fluoride,
- High pure reagent,
- Anions
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沈阳化工大学材料科学与工程学院沈阳 110142