• Application Note

EPA Method 331.0 Determination of Perchlorates in Drinking Water by Liquid Chromatography Electrospray Ionization Mass Spectrometry

EPA Method 331.0 Determination of Perchlorates in Drinking Water by Liquid Chromatography Electrospray Ionization Mass Spectrometry
  • Waters Corporation
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This is an Application Brief and does not contain a detailed Experimental section.

Abstract

This application brief demonstrates the determination of perchlorates in drinking water by Liquid Chromatography Electrospray Ionization Mass Spectrometry.

Introduction

Perchlorate is both naturally occurring and man-made. In its natural form, perchlorate is a contaminant in fertilizers. Man-made perchlorate is used in a wide variety of industrial applications including the production of rubber and paint, in lubricants, and as a primary ingredient in solid rocket propellant. Perchlorate is highly water soluble and can migrate into groundwater and surface water, posing a concern to drinking water supplies. Thirty-five states have detected perchlorate in drinking water at higher levels than expected. The United States Environmental Protection Agency (US EPA) has established an official reference of 0.0007 ppb per day of perchlorate. Maryland, Massachusetts, and New Mexico have established a one part per billion (ppb) action limit, while California and Texas have established 4 ppb limits.

Experimental

HPLC Conditions

Instrument:

Waters Alliance HPLC and Conductivity DSetector

Eluent:

25 mM ammonium bicarbonate, pH = 10 in 50% acetonitrile

Column:

Waters IC-Pak A/HR, 4.6 x 150 mm, 7 μm @ 30 °C

Injection:

100 μL

Flow Rate:

0.5 mL/min

Data:

Waters MassLynx Software

MS Conditions

Instrument:

Waters TQ Detector or Quattro micro API Mass Spectrometer

Ion Mode:

Electrospray negative (ESI-)

Mode:

Multiple reaction monitoring (MRM). The MRM transitions, cone voltages (CV) and collision energies (CE) are listed below.
Optimized MRM transition parameters for EPA method 331.0 in ES-.
Optimized MRM transition parameters for EPA method 331.0 in ES-.

Sample Preparation

No sample pretreatment. Add internal standard.

1 ppb perchlorate in HTDS.
1 ppb perchlorate in HTDS.
Perchlorate detection.
0.5 ppb perchlorate detection in three different sample matrices by LC-MS/MS. Analyzed on consecutive days with fresh eluent.

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