Method Statement Sulphide

@(#) Uncontrolled Document sulphide.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.

This procedure describes the determination of sulphide in soils and waters by distillation using appropriate reagents followed by a colorimetric measurement at 665nm.

Principle

Sulphides are decomposed by steam distillation using sodium hydroxide. The sulphide liberated is trapped in a solution of dilute sodium hydroxide and measured colorimetrically at a wavelength of 665 nm after addition of sulphuric acid, N,N-Diethyl-p-phenylenediamine sulphate and potassium dichromate to an aliquot of the distillate.

Performance Characteristics

Substances Determined

Sulphide in soils and waters.

Range of Application

  • Soil samples 10 to 100 mg / kg

  • Aqueous samples 0.05 to 0.5 mg / l

Limit of Detection

  • Solid samples 10 mg / kg

  • Aqueous samples 0.05 mg / 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

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

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