Sulfur determination in petroleum and petroleum products ASTMD 4294-98

The standard is identical to ASTMD 4294-98 «Petroleum and petroleum products. Determination of sulfur by method of energy-dispersive X-ray fluorescence spectrometry».
This test method covers the measurement of sulfur in hydrocarbons, such as diesel, naphta, kerosene, residuals, lubricating base oils, hydraulic oils, jet fuels, crude oils, gasoline (all unleaded), and other discillates containing 85% and 100% of methanol.
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No sample preparation for analysis is required.
The sample in a sample cup is exposed to primary X-ray tube emission in spectrometer. Countrate of S-Kα emission is measured. Background radiation is measured on  a blank sample containing no sulfur. Intensity without background is calculated. Sulfur content is determined with calibration curve for the given concentration range.
The test method provides sulfur determination in the range from 0,0150 % up to 5,00 % with the following precision parameters:

Repeatability, r
The difference between successive test results obtained by the same operator with the same apparatus under constant operation conditions on identical test material would, in the long run, in normal and correct operation of the test method exceed the following values only on case in twenty.
r = 0.02894 (X + 0,1691),
where  X is sulfur concentration in mass  %.

Reproducibility R
The difference between two single and independent results obtained by different operators working in different laboratories on identical test material would, in the long run, in normal and correct operation of the test method exceed the following values in one case in twenty.
R = 0.1215 (Х + 0,05555),
where  X is sulfur concentration in mass  %.

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