1994
DOI: 10.1021/ac00087a015
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Determination of Sulfur in Fossil Fuels by Isotope Dilution Thermal Ionization Mass Spectrometry

Abstract: Total sulfur has been measured in 13 petroleum and 14 coal Standard Reference Materials (SRMs) by isotope dilution thermal ionization mass spectrometry. These materials are suitable as primary and quality control standards for determining the sulfur content of oils and coals by X-ray fluorescence and high-temperature combustion instrumentation. Samples were spiked with enriched stable 3% and combusted in sealed Carius tubes using nitric and hydrochloric acids. The oxidized sulfur was reduced to HzS, precipitat… Show more

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Cited by 40 publications
(23 citation statements)
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“…The sulfur isotope ratio δ 34 S measurement using MC‐TIMS is performed by determination of the polyatomic ions 75 As 32 S + and 75 As 34 S + . The main advantage of this technique is that a very small sample mass is needed (a minimum mass of 0.2 µg S) . However, sample preparation for this method is also complex and time‐consuming.…”
Section: Main Isobaric Interferences On Sulfur Isotope Massesmentioning
confidence: 99%
“…The sulfur isotope ratio δ 34 S measurement using MC‐TIMS is performed by determination of the polyatomic ions 75 As 32 S + and 75 As 34 S + . The main advantage of this technique is that a very small sample mass is needed (a minimum mass of 0.2 µg S) . However, sample preparation for this method is also complex and time‐consuming.…”
Section: Main Isobaric Interferences On Sulfur Isotope Massesmentioning
confidence: 99%
“…Since the 1990s the certification of sulfur in fossil fuels and other matrices at the National Institute of Standards and Technology (NIST, Gaithersburg, MD, USA) has been exclusively performed using isotope dilution thermal ionization mass spectrometry (ID‐TIMS). While this method gives precise and accurate values for materials with moderate to high sulfur concentrations, it is limited in its capability for very low concentration measurements (<1 µg/g) due to the blank associated with the chemical reduction procedure; typically 0.2 S µg …”
Section: Isobaric Inteferences On the Sulfur Isotope Massesmentioning
confidence: 99%
“…Since the 1990s the certification of sulfur in fossil fuels and other matrices at the National Institute of Standards and Technology (NIST, Gaithersburg, MD, USA) has been exclusively performed using isotope dilution thermal ionization mass spectrometry (ID-TIMS). While this method gives precise and accurate values for materials [1][2][3][4][5] with moderate to high sulfur concentrations, it is limited in its capability for very low concentration measurements (<1 mg/g) due to the blank associated with the chemical reduction procedure; typically 0.2 S mg. [1][2][3][4][5] In recent years, inductively coupled plasma mass spectrometry (ICP-MS) has been investigated as a means of measuring the sulfur amount of lower concentration materials. [6][7][8][9][10][11][12][13] The main advantage of ICP-MS techniques over ID-TIMS is the elimination of the chemical reduction procedure needed for the latter technique.…”
mentioning
confidence: 99%
“…The venting process should be conducted behind an appropriate explosion-resistant safety shield by appropriately trained personnel. A discussion of Carius tube design for minimizing losses and hazards by explosion has been provided by Gordon et al [14] and references therein to their two previous papers and also in more recent work [15,16].…”
Section: Safety Considerationsmentioning
confidence: 99%