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New Methods for Measurement of Sulfur in Fossil Fuels


The Environmental Chemical Sciences Group has developed isotope dilution microwave induced combustion sector-field inductively coupled plasma mass spectrometry (ID-MIC-SF-ICP-MS) as a new measurement method for the determination of sulfur in coals.


Schematic illustration showing a device with a microwave source, central flame with sample introduction by syringe in the presence of oxygen, nitric acid, and hydrogen peroxide.

Graphical depiction of the microwave induced combustion process for sulfur determination in coal SRMs

Credit: NIST

NIST has a long history of developing high accuracy analytical methods and SRM materials for trace elements in fossil fuels.  NIST has applied the microwave induced combustion methodology in combination with isotope dilution analysis for sulfur determinations, representing the first-reported combination of this robust sample preparation methodology and high-accuracy quantification approach. Medium-resolution mode sector-field inductively coupled plasma mass spectrometry is utilized to avoid spectral interferences on the sulfur isotopes. 

Associated Publications 

1. Mossner, S. G. and Wise, S. A., "Determination of polycyclic aromatic sulfur heterocycles in fossil fuel-related samples," Analytical Chemistry, 71, 58-69 (1999). 

2. Yu, L. L., Kelly, W. R., Fassett, J. D., and Vocke, R. D., "Determination of sulfur in fossil fuels by isotope dilution electrothermal vaporization inductively coupled plasma mass spectrometry," Journal of Analytical Atomic Spectrometry, 16, 140-145 (2001). 

3. Kelly, W. R., Mann, J. L., Turk, G. C., and Vocke, R. D., "Determination of sulfur in ultra-low sulfur diesel fuel: Current status based on an international comparison," Abstracts of Papers of the American Chemical Society, 230, U210 (2005). 

4. Mann, J. L., Vocke, R. D., and Kelly, W. R., "Determination of low-level (sub-microgram) sulfur concentrations by isotope dilution multi-collector inductively couple plasma mass spectrometry using a 33S spike and internal normalization for mass bias correction," Rapid Communications in Mass Spectrometry, 26, 1175-1180 (2012). 

5. Zeigler, C., Schantz, M., Wise, S., and Robbat, A., "Mass Spectra and Retention Indexes for Polycyclic Aromatic Sulfur Heterocycles and Some Alkylated Analogs," Polycyclic Aromatic Compounds, 32, 154-176 (2012). 

6. Amais, R. S., Long, S. E., Nobrega, J. A., and Christopher, S. J., "Determination of trace sulfur in biodiesel and diesel standard reference materials by isotope dilution sector field inductively coupled plasma mass spectrometry," Analytica Chimica Acta, 806, 91-96 (2014). 

7. Paul, R. L., "Prompt gamma-ray activation analysis for certification of sulfur in fuel oil SRMs," Journal of Radioanalytical and Nuclear Chemistry, 311, 1149-1154 (2017). 

Created October 5, 2016, Updated October 30, 2023