This document describes the procedures and the precautions to be taken in drawing representative samples of ethylene in the liquid phase stored at -100 °C and in the gaseous phase, for the purpose of their analysis. Annex A sets out a diagrammatic representation of a system for the disposal of the portion of the sample which is not used in the analysis.

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This document describes the procedures and precautions to be taken in drawing representative samples of propylene and butadiene, in the liquid phase, for the purpose of their analysis. Annex A sets out a diagrammatic representation of a system for the disposal of the portion of the sample not used in the analysis. Annexes B, C and D show the sequence of operations for filling a sampling cylinder in non-closed and closed sampling apparatus.

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The method comprises the passage of a gaseous test portion through water to absorb acetone, acetonitrile, propan-2-ol and methanol, and subsequent gas chromatographic analysis of the aqueous solution, using a flame ionization detector, and comparison of the peaks obtained with those derived from an external standard. The method is applicable to products having acetone, propan-2-ol and methanol concentrations greater than 1 mg/kg, and acetonitrile concentrations greater than 10 mg/kg.

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Gives methods for the determination of water using an analyzer with an in-line sensor in gaseous flows of the substance to be analyzed. Compiles the various principles of working of the most generally used commercial analyzer like electrolytic decomposition - light reflection on a cooled mirror (dew-point) - modification of vibration frequency of a quartz crystal covered with a hygroscopic layer - variation of the capacity of a capacitor formed by a hygroscopic dielectric polymer and two porous electrodes - infrared spectrometry - Micro-wave absorption measurement - variation of the capacity of a capacitor consisting of an aluminium oxide dielectric covered by an evaporated porous gold film.

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Specifies a method of sampling by scrubbing at dry ice temperature (195 K). Permits the concentration of traces of all the less volatile polar compounds (water, alcohols, esters, acids, amines, etc.) in a small amount of liquid phase practically without any interference due to adsorption phenomena on the relatively small internal surfaces of the scrubbing absorber. This sampling technique permits the exact determination of all these polar compounds at contents greater than 0.01 mg/m^3, at normal temperature and pressure. Is also applicable to the determination of hydrocarbons with a higher boiling point (for example traces of oil in ethylene).

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A gaseous or liquid test portion is aspirated into the oxygen-hydrogen flame of a burner where it is burned with considerable excess of oxygen. the liberated chlorine and hydrochloric acid are absorbed in hydrogen peroxide solution. The chloride ions are conductimetrically or potentiometrically titrated with a silver nitrate solution.

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Describes the procedure and the precautions to be taken in drawing representative samples of the substances for the purpose of their analyses. It also sets out, in Annex A, a diagrammatic representation of a system for the disposal of the portion of the sample not used in the analysis, and, in Annex B, the sequence of operations for filling a sample cylinder.

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After sampling and preparation of the laboratory sample the gaseous test portion is passed at a given rate through an electrochemical cell previously calibrated with air or with standard mixtures containing a known amount of oxygen, and the concentration of oxygen in the gaseous olefin is measured. The method is applicable to light olefins having an oxygen content greater than 1 milliliter per cubicmeter.

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Describes the procedure and the precautions to be taken in drawing representative samples of ethylene in the liquid phase stored at -100 °C and in the gaseous phase, for the purpose of their analysis excluding the determination of water content, other polar components and hydrocarbons heavier than C5. In an annex a diagrammatic representation is given of a system for the removal of the portion of the sample not used in the analysis.

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A liquid or a vaporized gaseous test portion is injected into a gas chromatography column. After passage of the test portion through this column the oligomers are separated. The detection is performed by flame ionization. The peaks obtained are compared with those derived from an external standard. The oligomers which may be present are: 4-vinyl cyclohexene, 1,3-cyclooctadiene, 1,5-cyclooctadiene. The method is applicable to butadiene having oligomer contents greater than 10 mg/kg.

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A liquid sample obtained at low temperature is vaporized and then passed through a chromatographic column which permits the separation of the oligomers. The detection is performed by flame ionization an the peaks obtained are compared with those derived from an external standard. The method is applicable to propylene having propene dimers (hexenes) contents greater than 20mg/kg and propene trimers (nonenes) contents greater than 30 mg/kg.

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The active TBC in a test portion is extracted by mixing with a solution containing m-nitrophpenol (as the internal standard) and evaporating the butadiene. The TBC and m-nitrophenol are separated by high-performance liquid chromatography and detected by UV: The peak areas or peak heights are measured and the TBC content is determined by using a calibration graph. The polymerization inhibitor TBC can also be determined by a spectrometric method (ISO 6684) but that method is not able to differentiate between the active inhibitor and its oxidized, inactive form. The present method specifically measures the concentration of the active form of TBC. The method is applicable to butadiene having TBC contents in the range 0 to 250 mg/kg.

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TBC is added as an oxidation inhibitor to 1,3-butadiene for industrial use. For the determination the inhibitor is separated from the butadiene by evaporation. The residue is dissolved in water and an excess of iron(III) chloride is added. The spectrometric measurement of the absorbance of the yellow-coloured complex is carried out at a wavelength of about 425 nm. The method is applicable to butadiene containing more than 50 mg TBC per kilogram.

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The analysis is carried out with a gas chromatograph fitted with a thermal conductivity detector. It can be operated at two temperatures, either at - 78 degrees centigrade or at ambient temperature. At ambient temperature, oxygen and argon are not separate and the method thus only allows the total content of these two gases to be determined. When the operations are carried out at - 78 degrees centigrade, these two gases are separated.

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A test solution is treated with an excess of acidified potassium bromide-bromate solution in the presence of mercury(II) sulphate. After addition of potassium iodide solution the liberated iodine is titrated with standard volumetric sodium thiosulphate solution.

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Covers a method based on the selection of a gas chromatography column allowing the separation of the impurities to be determined. A gaseous test portion is passed through this column and the peaks obtained are detected by flame ionization and compared with those derived from an external standard. Uses two types of columns, one for the determination of methane, ethane and acetylene (adsorption chromatography) and the other for the determination of the other impurities (gas/liquid partition chromatography).

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Describes a method based on the separation of carbon monoxide, methane and corbon dioxide by gas chromatography through a Carbosieve B or Porapak N column, followed by passage through a column of hydrogenation catalyst which transforms the oxides of carbon to methane thus allowing the use of a flame ionization detector to make the final determination.

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Covers a method based on the selection of a gas chromatography column allowing the separation of the impurities to be determined. A gaseous test portion is passed through this column and the peaks obtained are detected by flame ionization and compared with those derived from an external standard. Columns and operating conditions having been found suitable for such a test are indicated in Annex A while Annex B lists the absolute retention times indicated in minutes. Annex C includes a typical chromatogram from an alumina column.

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Covers a method based on the selection of a gas chromatography column allowing the separation of the impurities to be determined. A gaseous test portion is passed through this column and the peaks obtained are detected by flame ionization and compared with those derived from an external standard. Columns and operating conditions having been found suitable for such a test are indicated in Annex A while Annex B lists the absolute retention times with regard to the analysis of butadiene. Annex C includes a typical chromatogram from a Sebaconitrile column.

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Relates particularly to ethylene (ethene), propylene (propene) and butadiene (1,3-butadiene). Lists the apparatus to be used, describes sampling and procedure and provides information on the expression of results and the data to be included in the test report.

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A test portion is treated with a solution of bromine in absolute methanol saturated with sodium bromide (Kaufman solution). After addition of potassium iodide solution the liberated iodine is titrated with standard volumetric sodium thiosulfate solution. The degree of unsaturation is expressed as iodine value, the number of grams of iodine absorbed by 100 g of a substance under specified conditions of test.

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Describes a method applicable to products having water contents between 10 and 100 mg/kg. Specifies the manner of applications of the Karl-Fischer method, whose principle and chemical reaction are given in ISO 760 which should also be used for higher water contents as sampling is not valid when there is a risk that condensation of water may occur. The principle consists in absorbing the traces of water in a test portion in a solvent to which a sufficient quantitty of Karl-Fischer reagent has been added so that there is neither an excess of water nor an excess of the Karl Fischer reagent, when the solvent is said to be at the equivalence point.

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Covers a method applicable to products having ammonia contents greater than 0,25 mg/kg. Consists in absorbing the ammonia from a gaseous sample in sulphiric acid medium with the formation of ammonium sulphate and passing a current of nitrogen into the absorption liquid to remove hydrogen sulphide which would interfere. This is followed by formation in an alkaline medium of the indophenol complex by reaction of the ammonium ions with phenol and hypochlorite ions in the presence of sodium pentacyanonitrosoferrate(III) as catalyst, and photomeric measurement of the blue coloration obtained at a wavelength of about 625 nm.

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