Sulfur determination in petroleum products GOST R EN ISO 14596-2008

The standard is identical to EN ISO 14596:1998 «Petroleum products - Determination of sulfur content - Wavelength-dispersive X-ray fluorescence spectrometry».
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ISO 14596 specifies a method for the determination of the sulfur content of liquid petroleum products, additives for petroleum products, and semi-solid and solid petroleum products that are either liquefied by moderate heating or soluble in organic solvents of negligible or accurately known sulfur content.
The test material is mixed with internal standard (zirconium solution) in a given mass proportion, put in a sample cup and exposed to an X-ray tube primary radiation.
Countrate of S-Kα emission at wavelength 0.5373, count rate of ZrLα1 at wavelength 0.6070 nm is measured. Background radiation is measured at 0.545 nm. Relations between these counrates are calculated.. Sulfur content is determined with calibration curve obtained with calibration standards for the given concentration range.
The method is applicable to products or additives having sulfur contents in the range 0,001 % (m/m) to 2,50 % (m/m); higher contents can be determined by appropriate dilution. Other elements do not interfere at concentrations anticipated in the materials subject to this analysis.

Precision parameters
Repeatability

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.

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.

Table: Precision parameters in mass %
Sulfur contentRepeatabilityReproducibility
From 0.0010 up to  0.00290,00030,0005
From 0.0030 up to 0.0049
0,00060,0010
From 0.0050 up to 0.00990,00100,0020
From 0.010 up to 0.029
0,0020,005
From 0.030 up to 0.0490,0030,005
From 0.050 up to 0.099
0,0050,010
From 0.10 up to 0.990,010,20
From 1.00 up to 2.500,020,04

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