BS EN ISO 3924:2016 pdf download – Petroleum products — Determination of boiling range distribution — Gas chromatography method (ISO 3924:2016)
If stationary phases other than those listed in the note in 5.1 are used, the retention times of a few alkylbenzenes across the boiling range such as o-xylene, n-butylbenzene, 1,3,5-tri-isopropylbenzene, n-decylbenzene and n-tetradecylbenzene shall also be checked to make certain that the column is separating according to the boiling point order (see Annex C). 5.7 Reference material, the primary reference material used shall be the ASTM Reference Gas Oil No.1. 5.8? Carbon? disulfide, reagent grade (CAS RN 75-15-0).
6 Apparatus
6.1 Chromatograph, any gas chromatograph that has the following performance characteristics may be used.
6.1.1 Detector, of either the flame ionization or thermal conductivity type. The detector shall have sufficient sensitivity to detect a mass fraction of 1,0 % of dodecane with a peak height of at least 10 % of full scale on the recorder under the conditions specified in this International Standard, and without loss of resolution as defined in 8.3. When operating at this sensitivity level, detector stability shall be such that a baseline drift of not more than 1 % of full scale per hour is obtained. The detector shall be capable of operating continuously at a temperature equivalent to the maximum column temperature employed. The detector shall be connected to the column in such a way that any cold spots between the detector and the column are avoided. NOTE It is not desirable to operate thermal conductivity detectors at a temperature higher than the maximum column temperature employed. Operation at higher temperatures only serves to shorten the useful life of the detector, and generally contributes to higher noise levels and greater drift.
6.1.2 Column temperature programmer, capable of programmed temperature operation over a range sufficient to establish a retention time of at least 1 min for the initial boiling point and to elute the entire sample within the temperature ramp. The programming rate shall be sufficiently reproducible to obtain retention time repeatability of 6 s for each component in the calibration mixture (5.6). If the initial boiling point is less than approximately 93 °C, an initial column temperature below ambient can be required. However, excessively low initial column temperatures shall be avoided, to ensure that the stationary phase remains liquid. The initial temperature of the column shall be only low enough to obtain a calibration curve meeting the requirements of this International Standard.
6.1.3 Sample inlet system, either be capable of operating continuously at a temperature equivalent to the maximum column temperature employed or provide on-column injection with some means of programming the entire column, including the point of sample introduction, up to the maximum temperature required. The sample inlet system shall be connected to the chromatographic column in such a way that any cold spots between the inlet system and the column are avoided. 6.2 Column, any column and conditions may be used, provided that, under the conditions of the test, separations are in the order of boiling points as given in Table 1, and the column resolution, CR, is at least 3 (8.3). Typical column operating conditions are given in Table 2 and 3.
6.3 Recorder/plotter, this apparatus is used for plotting the chromatogram. This may be accomplished using a 0 mV to 1 mV recording potentiometer having a full-scale response time of 2 s or less and a minimum chart width of approximately 120 mm. Alternatively, a computer or other device may be used, provided it is capable of graphics presentation of the same or better quality as a potentiometric recorder.
6.4 Integrator/computer, this apparatus is used for determining the accumulated area under the chromatogram. This may be achieved by using a computer-based chromatography data system or an electronic integrator. BS EN ISO 3924 pdf download.