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Journal of Chromatography A
Volume 1118, Issue 1, 16 June 2006, Pages 100-105
18th Annual International Ion Chromatography Symposium
 
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doi:10.1016/j.chroma.2006.01.138    How to Cite or Link Using DOI (Opens New Window)
Copyright © 2006 Elsevier B.V. All rights reserved.

Determination of perchlorate in drinking water by ion chromatography using macrocycle-based concentration and separation methods

John D. LambCorresponding Author Contact Information, a, E-mail The Corresponding Author, David Simpsona, Bryce D. Jensena, Joseph S. Gardnera and Quinn P. Petersona

aDepartment of Chemistry and Biochemistry, Brigham Young University, C-100 BNSN, Provo, UT 84602, USA

Available online 3 March 2006.

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Abstract

Macrocycle-based ion chromatography provides a convenient, reliable method for the determination of perchlorate ion, which is currently of great interest to the environmental community. This study shows that effective perchlorate determinations can be made using standard conductimetric detection by combining an 18-crown-6-based mobile phase with an underivatized reversed-phase mobile phase ion chromatography (MPIC) column. One unique feature of this method is the flexibility in column capacity that is achieved through simple variations in eluent concentrations of 18-crown-6 and KOH, facilitating the separation of target analyte anions such as perchlorate. Using a standard anion exchange column as concentrator makes possible the determination of perchlorate as low as 0.2 ug/L in low ionic strength matrices. Determination of perchlorate at the sub-ug/L level in pure water and in spiked local city hard water samples with high background ion concentrations can be achieved this way. However, like other IC techniques, this method is challenged to achieve analyses at the ug/L level in the demanding high ionic strength matrix described by the United States Environmental Protection Agency (EPA) (1000 mg/L chloride, sulfate and carbonate). We approached this challenge by use of the Cryptand C1 concentrator column, provided by Dionex Corporation, to effectively preconcentrate perchlorate while reducing background ion concentrations in the high ionic strength matrix. The retention characteristics of the concentrator column were studied in order to maximize its effectiveness for perchlorate determinations. The method makes possible the determination of perchlorate at the 5 ug/L level in the highest ionic strength matrix described by the EPA.

Keywords: Ion chromatography; Crown ether; 18-crown-6; Perchlorate; Trace level detection; EPA Method 314.1; Cryptand concentrator

Article Outline

1. Introduction
2. Experimental
2.1. Materials
2.2. Instrumentation
3. Results and discussion
3.1. Effect of mobile phase 18-crown-6 on retention of polarizable anions
3.2. Analyte targeting
3.3. Optimization for perchlorate
3.4. Low level perchlorate determinations
3.5. Matrix elimination
3.6. Application to real water samples
3.7. EPA standard samples
3.7.1. Analysis of Cryptand C1 concentrator
3.7.2. Trace perchlorate and the EPA high salt standard
4. Conclusions
Acknowledgements
References







Journal of Chromatography A
Volume 1118, Issue 1, 16 June 2006, Pages 100-105
18th Annual International Ion Chromatography Symposium
 
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