ASTM D6349

Determination of Major and Minor Elements in Coal, Coke, and Solid Residues from Combustion of Coal and Coke by Inductively Coupled Plasma- Atomic Emission Spectrometry

Applicability: This procedure applies to coal, coke, and solid residues from combustion of coal and coke received by Conti Testing Laboratories, Inc. (CTL), Pittsburgh, Pennsylvania. These residues may be laboratory ash, bottom ash, fly ash, flue gas desulfurization sludge, and other combustion process residues. The analyst must be specially trained and experienced in spectral interpretations prior to operating this instrument or determining concentrations by this method.
1.1. Method Reference: ASTM D6349
1.2. Scope and Application:
1.2.1. Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES) may be used to determine major and minor elements in coal, coke, and solid residues from combustion of coal and coke. The solid residues may be laboratory ash, bottom ash, fly ash, flue gas desulfurization sludge, and other combustion process residues. All solid matrices require acid digestion prior to analysis.

Purpose: The purpose of this procedure is to provide a method for the determination of metals in solid samples. Inductively coupled plasma-optical emission spectrometry (ICP-OES) is used to determine metals in solution after acid digestion. The analysis described in this method involves multi-elemental determinations by ICP- OES. The instrument measures characteristic atomic-line emission spectra by optical spectrometry. Samples are nebulized and the resulting aerosol is transported to the plasma torch. Element specific emission spectra are produced by radio-frequency inductively coupled plasma. The spectra are dispersed by a grating spectrometer, and the intensities of the line spectra are monitored at specific wavelengths by a photosensitive device. Photocurrents from the photosensitive device are processed and controlled by a computer system. A background correction technique is required to compensate for variable background contribution to the determination of the analytes. Background must be measured adjacent to the analyte wavelength during analysis. The position selected for the background-intensity measurement, on either or both sides of the analytical line, will be determined by the complexity of the spectrum adjacent to the analyte line. The position used should be as free as possible from spectral interferences and should reflect the same change in background intensity as occurs at the analyte wavelength measured.