Method Statement 2:1 Sulphate

@(#) Uncontrolled Document 2to1sulphate.html Version 1.1 Last Revised on 12/09/02




Contents

Introduction

Principle

Performance Characteristics

Range of Application

Limit of Detection

Analytical Quality Control

References

Introduction

The performance of this method is validated in accordance with internationally recognised procedures.

The analytical procedure described herein outlines the determination of water soluble sulphate in soils by Inductively Coupled Plasma – Optical Emission Spectrophotometry (ICP-OES).

Principle

Soil samples are leached at a water:soil ratio of 2:1. The filtered extracts are aspirated into a plasma torch. Measurement of the atomic emission of the element is made by an optical spectroscopic technique. Samples are nebulised and the aerosol produced is transported to a plasma torch where excitation occurs. Characteristic atomic-line emission spectra are produced by a radio-frequency inductively coupled plasma. The spectra are dispersed by a grating spectrometer and intensities of the lines are monitored by photomultiplier tubes. The photocurrents from the photomultiplier tubes are processed and controlled by a computer system.

Performance Characteristics

Substances Determined

Water soluble Sulphate (2:1 leachate). Note that results are normally reported in units of g/l upon the 2:1 leachate.

Range of Application

  • Soil samples 0.1 to 100 g/l

Limit of Detection

  • Soil samples 0.1 g / l

Analytical Quality Control

Analytical quality control is maintained by a number of measures:

  • Multi-point calibration with authentic standards (with defined minimum performance characteristics)

  • Analysis of control samples within each analytical batch, such as independent standards, matrix spikes or reference materials

  • Analysis of reagent/method blanks within each analytical batch

  • Ongoing quality assured by the use of control charts in conjunction with warning and action limits for the QC sample data

  • Participation in external proficiency testing and interlaboratory schemes such as LGC CONTEST, HSE WASP, CSL FAPAS

References

A Handbook of Inductively Coupled Plasma Spectrometry. M. Thompson, J.N.. Walsh. 1983. ISBN 0-412-00371-6)

Standard Methods for the Examination of Waters and Wastewaters. APHA-AWWA-WEF, 1992 18th Edition



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