Rapid analysis of perchlorate, chlorate and bromate ions in concentrated sodium hypochlorite solutions

Aleksey N. Pisarenko, Benjamin D. Stanford, Oscar Quiñones, Gilbert E. Pacey, Gilbert Gordon, Shane A. Snyder

Research output: Contribution to journalArticlepeer-review

38 Scopus citations

Abstract

A sensitive, rapid, and rugged liquid chromatography with tandem mass spectrometry (LC-MS/MS) method for measuring concentrations of perchlorate, chlorate, and bromate ions in concentrated sodium hypochlorite solutions is presented. The LC-MS/MS method offers a practical quantitation limit (PQL) of 0.05 μg L-1 for ClO4-, 0.2 μg L-1 for BrO3-, and 0.7 μg L-1 for ClO3- and a sample analysis time of only 10 min. Additionally, an iodometric titration technique was compared with the LC-MS/MS method for measurement of chlorate ion at high concentration. The LC-MS/MS method was the most reproducible for chlorate concentrations below 0.025 M while the iodometric titration method employed was the most reproducible above 0.025 M. By using both methods, concentrations of chlorate can be measured over a wide range, from 0.7 μg L-1 to 210 g L-1 in hypochlorite ion solutions. Seven quenching agents were also evaluated for their ability to neutralize hypochlorite ion, thereby stopping formation of perchlorate ion in solution, without adversely impacting the other oxyhalide ions. Malonic acid was chosen as the quenching agent of choice, meeting all evaluation criteria outlined in this manuscript.

Original languageEnglish (US)
Pages (from-to)216-223
Number of pages8
JournalAnalytica Chimica Acta
Volume659
Issue number1-2
DOIs
StatePublished - Feb 5 2010
Externally publishedYes

Keywords

  • Bromate ion
  • Chlorate ion
  • Malonic acid
  • Perchlorate ion
  • Sodium hypochlorite

ASJC Scopus subject areas

  • Analytical Chemistry
  • Biochemistry
  • Environmental Chemistry
  • Spectroscopy

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