BS EN 13132 pdf free download
BS EN 13132 pdf free download.Liquid petroleum products一Un leaded petrol – Determination of organic oxygenate compounds and total organically bound oxygen content by gas chromatography using column switching.
3 Principle Oxygen containing organic compounds are isolated from the sample using a first capillary column. In a second capillary column the oxygen containing organic compounds are separated, and detected individually using a flame ionization detector. NOTE Guidance on the column switching technique is given in annex B. 4 Reagents and materials Use only reagents of recognized analytical grade and water conforming to grade 3 of EN ISO 3696. 4.1 Carrier gas Hydrogen, helium, or nitrogen, free of hydrocarbons. WARNING Hydrogen is explosive when mixed with air at concentrations ranging approximately from 4 % (VM) to 75 % (VM). All joints and lines carrying hydrogen shall be made gas tight to prevent leakage of hydrogen into a confined space.4.3 Internal standards Use one of the reagents listed in 4.2. If all of these reagents are likely to be present in the sample under test, use a different organic oxygenate compound of the same purity and similar volatility. 4.4 Petrol containing no organic oxygenate compounds, or n-heptane Petrol which has been examined to ensure that it contains no organic oxygenate compounds detectable by this method, or n-heptane. 5 Apparatus Usual laboratory apparatus and glassware, together with the following: 5.1 Gas chromatographic assembly 5.1.1 Gas chromatograph, provided with a means for column switching, equipped with a programmable oven temperature controller, or controllers in the case of dual oven gas chromatographs, and a flame ionization detector (FID). NOTE It is recommended that a system constructed entirely of glass from the sample injection port up to the detector system is used since petrol may contain organic oxygenate compounds which can give rise to corrosion and changes of retention times in systems constructed using metals.6 Sampling Unless otherwise specified in the commodity specification, samples shall be taken in accordance with EN ISO 3170 or EN ISO 3171, and/or in accordance with the requirements of national standards or regulations for the sampling of petrol. 7 Procedure 7.1 Setting up the apparatus 7.1.1 General Prepare the equipment and set the test conditions in accordance with the manufacturer’s instructions. 7.1.2 Carrier gas Adjust the pressure and flow rate of the carrier gas to levels such that the resolutions are in accordance with 5.1.2. 7.2 Calibration Prepare the calibration sample by combining known masses of organic oxygenate compounds (4.2), with the internal standard (4.3), and diluting them to a known mass with the petrol or n-heptane (4.4). .NOTE The calibration sample should contain the same organic oxygenate compounds in similar proportions as present in the sample under test. Inject a suitable quantity of the prepared calibration sample into the gas chromatograph such that the capacity of the columns and other components is not exceeded and the linearity of the detector is not impaired.7.4 Preparation of test sample Cool the sample to between 5 °C and 10 °C. Weigh, to the nearest 0,1 mg, the test sample container (5.3) and its rubber septum without sealing it. Transfer a quantity of the internal standard (4.3) to the test sample container and weigh, to the nearest 0,1 mg, the test sample container with contents and septum, without sealing the sample container. The mass, mst, in grams, of the internal standard shall amount to between 2 % (m/m) and 5 % (m/m) of the sample, ms, but shall not be less than 0,050 g. Transfer a quantity, normally between 5 ml and 100 mI, of the cooled sample to the test sample container and seal immediately with the septum. Weigh, to the nearest 0,1 mg, the test sample container and contents. Record the mass, ms, in grams, of the test sample taken, to the nearest 0,1 mg. Record the amount of internal standard in the prepared test sample as a percentage by mass. Mix the contents of the test sample container by shaking until homogeneous.BS EN 13132 pdf download.
