STP747

    Isotope Dilution Spark Source Mass Spectrometric Determination of Sulfur in Selected NBS Iron-Base Alloys

    Published: Jan 1981


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    Abstract

    A procedure has been developed at the National Bureau of Standards utilizing isotope dilution spark source mass spectrometry (ID-SSMS) for the determination of sulfur in iron-base alloys. With this technique a known amount of highly enriched sulfur-34 (34S) isotope (spike) is added to the sample, and, after physical and chemical equilibration between the spike sulfur and the natural sulfur in the sample, the equilibrated sulfur is isolated by reduction to hydrogen sulfide (H2S) and precipitation as silver sulfide (Ag2S). The altered isotopic ratio of the sulfur (32S/34S) is then measured with the spark source mass spectrometer. The sulfur concentrations are calculated from the sample weight, spike weight, measured altered isotope ratio, and known isotopic abundance of 34S and 32S in both the natural and spike sulfur. The key step in obtaining a quantitative sulfur analysis is the dissolution of the sulfur-containing iron samples in a sealed tube. This dissolution procedure enables the sample sulfur and the spike sulfur to equilibrate completely without any possibility of loss of either species by volatilization.

    Keywords:

    trace sulfur, isotope dilution spark source mass spectrometry, spark source mass spectrometry, sealed tube dissolution, NBS iron-base alloys, analytical techniques, trace constituents, metals


    Author Information:

    Paulsen, PJ
    Research chemists and physical science technician, National Measurement Laboratory Center for Analytical Chemistry, National Bureau of Standards, Washington, D.C.,

    Burke, RW
    Research chemists and physical science technician, National Measurement Laboratory Center for Analytical Chemistry, National Bureau of Standards, Washington, D.C.,

    Maienthal, EJ
    Research chemists and physical science technician, National Measurement Laboratory Center for Analytical Chemistry, National Bureau of Standards, Washington, D.C.,

    Lambert, GM
    Research chemists and physical science technician, National Measurement Laboratory Center for Analytical Chemistry, National Bureau of Standards, Washington, D.C.,


    Paper ID: STP28100S

    Committee/Subcommittee: E03.02

    DOI: 10.1520/STP28100S


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