• Applikationsbericht

EPA Method 6850.0 Determination of Perchlorate in Water, Soils and Solid Wastes using High Performance Liquid Chromatography/Electrospray Ionization/Mass Spectrometry (HPLC-ESI/MS)

EPA Method 6850.0 Determination of Perchlorate in Water, Soils and Solid Wastes using High Performance Liquid Chromatography/Electrospray Ionization/Mass Spectrometry (HPLC-ESI/MS)

  • Waters Corporation

This is an Application Brief and does not contain a detailed Experimental section.

Abstract

This application brief demonstrates the determination of perchlorate in water, soils and solid wastes using High Performance Liquid Chromatography/Electrospray Ionization/Mass Spectrometry (HPLC-ESI/MS).

Introduction

Perchlorate is both naturally occurring and man-made. In its natural form, perchlorate is a contaminent 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 dose 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 2695 System with Conductivity Detector

Column:

IC-Pak Anion HR, 6 μm , 4.6 x 75 mm

Eluent:

25 mM NH4HCO3, pH 10 with NH4OH in 50% ACN

Flow rate:

0.5 mL/min

Column temp:

30 °C

Back pressure:

<1000 psi

Back conditions:

~1600 μS

Injection:

100 μL

MS Conditions

Instrument:

Quattro micro Mass Spectrometer

Ionization:

ESI- LM 1 Resolution: 15

Capillary (V):

.58 HM 1 Resolution: 15

Cone (V):

40 Ion Energy 1: 0.6

Extractor (V):

3 Entrance (V): 1

RF Lens (V):

0.3 Collision Energy: 30

Source temp ˚C:

125 Exit: 1

Desolvation temp:

400 LM 2 Resolution: 14

Cone Gas (L/hr):

50 HM 2 Resolution: 14

Desolvation gas:

500 Ion Energy 2: 1

Gas cell pressure:

2 x 10-2 mbar Multiplier: 650

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