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SURVEY OF BOTTLED WATERS FOR PERCHLORATE BY ELECTROSPRAY IONIZATION MASS SPECTROMETRY (ESI-MS) AND ION CHROMATOGRAPHY (IC)
Citation:
Urbansky*, E T., B. Gu, M L. Magnuson*, G. M. Brown, AND C A. Kelty*. SURVEY OF BOTTLED WATERS FOR PERCHLORATE BY ELECTROSPRAY IONIZATION MASS SPECTROMETRY (ESI-MS) AND ION CHROMATOGRAPHY (IC). JOURNAL OF THE SCIENCE OF FOOD AND AGRICULTURE. John Wiley & Sons, Ltd., Indianapolis, IN, 80(12):1798-1804, (2000).
Description:
Perchlorate has been identified in ground and surface waters around the US, including some that serve as supplies for drinking water. Because perchlorate salts are used as solid oxidants in rockets and ordnance, water contamination may occur near military or aerospace installations or defense industry manufacturing facilities. This ion has been added to the EPA's Contaminant Candidate List and the Unregulated Contaminant Monitoring Rule. Should EPA promulgate a regulation for municipal water systems, US law requires other agencies to take action on bottled water. Methods will therefore be required to determine perchlorate concentrations in not only tap water, but also bottled waters. Ion chromatography (IC) is the primary technique used for drinking water, but it does not provide a unique identification. Confirmation by electrospray ionization mass spectrometry (ESI-MS) can serve in this capacity. The ESI-M method can be applied to these products, but it requires an understanding of matrix effects, especially high ionic strength that can suppress electrospray. When using methyl isobutyl ketone (MIBK) as the extraction solvent, the ESI-MS method can reach lower limits of detection of 6 ng mL-1 for some bottled waters. However, dilution required to negate ionic strength effects in mineral waters can raise this by a factor of 10 or more, depending on the sample. Decyltrimethylammonium cation (added as the bromide salt) is used to produce an ion pair that is extracted into MIBK. After extraction, the sum of the peak areas of the ions C10H21NMe3(Br)(ClO4)-(m/z=380u) and C10H21NMe3(ClO4)2-(m/z=400u) isused to quantitate perchlorate. Standard additions are used to account for most of the matrix effects. In this work, five domestic brands and five imported brands of bottled water were comparatively analyzed by the two techniques. For comparison, a finished potable water known to contain perchlorate within the lower limit of detection for the IC method. Recoveries on spiked samples subjected to the IC method were > 98%.