BS EN 15199-2:2006 pdf download
BS EN 15199-2:2006 pdf download.Petroleum products – Determination of boiling range distribution by gas chromatography method – Part 2: Heavy distillates and residual fuels.
The end ol the test porhori is determined as given in A.6.
13 Calculation
Use the calculation protocol given in Annex A for the production of results,
14 ExpressIon of results
Report the tabulated results as follows:
a) report all temperatures to the nearest 1 ‘C:
b) report all percentages to the nearest 1 % (ni/rn):
C) report the 05 % (rn/rn) point as the initial boiling pont. and the recovery at selected final elution temperature (720 °C or 750 DC).
d) report intermediate percentages as required, at intervals of not less man 1 mm)
15 Precision
15,1 General
The precision was determined by statistical examination of inter-laboratory test results using EN ISO 4259 141
15.2 Repeatability
The difference between two test results, obtained by the same operator with the same apparatus under constant operating conditions on identical test material, would iithe long run in the normal and correct operation of the test method. exceed the values given in Table 3 only in one case in twenty.
15-3 ReproducIbility
The difference between two single and independent test results, Obtained by different operators working In different laboratories on identical test material, would in the long run, in the normal and correct operation of the test method, exceed the values given i Table 3 only in one case in twenty.
A.1 Application
The algorithm given in this Annex only applies for a slice width of 0,1 s to 0.2s (10 Hz to 5 Hz) The diromatogram for the reference material (5.9), the sample. and the baseline shall be zeroed The baseline dromatogram is subtracted from the Reference Material 5010 (5.9.2) and from the sample crwomalogram in order to obtain the net area. An extended procedure is given as informative guidance in Annex D.
A.2 Starting conditions
The following data are required for the commencement of calculations’
i) sample data array IN data points):
Ii) reference material data array (N data points).
iii) blank data array (N data points):
iv) processed data fite from calibration run with retention times of normal alkanes,
v) boiling points of normal alkanes used in calibration run:
vi) start sample time:
vii) end sample time
The data collection of the test portion or reference shall be identical to the used data points in the blank.
A.3 Zero sample or reference chromatogram
A.3.1 Subtract each blank slice area from me corresponding sample slice area.
A.3.2 Average the first twenty time slices from the subtracted slice areas.
A.3.3 Subtract the average slice area from each subtracted time slice to zero the chromatogram Set negative
numbers to zero,
A.4 Sample area
Calculate the total sample area by summing each of the corrected area slices
D.1 Zeroing of the reference material chromatogram
0.1.1 Examine the chromatogram obtained for Reference Material SOlO (5.9.2), and ensure, by visual inspection of the chromatogram in the data system. that the first 5 slices contain neither sample nor solvent elution
D.1 .2 Set up an array that contains slices obtained from the Reference Material 5010 chromatogram
Calculate the avef age of the first five area slices. Subtcact the average slice area from each slice in the
Reference Material 5010 chromatogram Set negative numbers to zero
Di .3 Zero the blank baseline chromatograni by carrying out an analogous calculation as in 0.1.2.
D.1 .4 Subtract the blank baseline from the Reference Material 5010 chromatogram Subtract each zeroed blank baseline slice from the corresponding zeroed Reference Material 5010 slice It there are negative slices set the slice values to zero
0.1.5 Determine me end of elution time of Reference Material 5010.
NOTE Since it is a requirement mat me sample chosen to obtain a response factor shall fully elute pro to the FEt time the end of sample elution for this chromatogram should be determined as described in EN 15199-1 1I. using the algorithm to determine the tine the signal of the completely eluted sample returns to basebie
D.1 .6 Determine the area of the chromatogram for Reference Material 5010 Determine the end twne of solvent elution Sum all of the slices from the end of solvent elution to the end of sample elution This is the area of the standard, Asm.
D.1 .7 Calculate the boiling point distribution of Reference Material 5010. The resulting corrected slices obtained for Reference Material 5010 are submitted to a calculation for boiling point distribution as in EN 15199-1 151. A comparison of the values obtained with the consensus values listed in Table 1 is made and all the boiling point values should fall within the specified windows. If this requirement is not met, correct any chromatographec problems pnor to proceeding with sampte analysis.
Typical problems found in this step are. contaminated solvent, problems in sample preparation. sample residue in the inlet or column. or both, quality of the baseline used. a partially blocked detector jet, or a combination thereof.
