ASTM_D_7845_-_13.pdf

Designation:D784513Standard Test Method forDetermination of Chemical Species in Marine Fuel Oil byMultidimensional Gas Chromatography MassSpectrometry1This standard is issued under the fixed designation D7845;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of last revision.A number in parentheses indicates the year of last reapproval.Asuperscript epsilon()indicates an editorial change since the last revision or reapproval.1.Scope1.1 This test method covers the quantitative determinationof a variety of chemical species in marine fuel oil(bunker fueloil)by gas chromatography mass spectrometry.By using thesame conditions and by selecting required mass spectralselected ions,the test method may be used for the determina-tion of other species than those for which precision statementsand limits of detection have been established.1.2 An example list of chemical species for which a limit ofquantification has been determined by means of this testmethod is given in Table 1.1.3 Other refinery hydrocarbon fractions and their mixturesmay be tested using the same test method conditions.However,the precision of this test method reflects the compounds inTable 1.1.4 Results are reported to the nearest 1.0 mg/kg.1.5 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.6 This standard does not purport to address all of thesafety concerns,if any,associated with its use.It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:2D4307 Practice for Preparation of Liquid Blends for Use asAnalytical StandardsD6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System Performance3.Terminology3.1 Definitions:3.1.1 direct or open split interface,nany GC/MS interfaceused to maintain atmospheric pressure at capillary columnoutlet.3.1.2 reconstructed ion chromatogram(RIC),na limitedmass chromatogram representing the intensities of ion massspectrometric currents for only those ions having particularmass to charge ratios used in this test method to selectivelyextract and identify components in the presence of a complexhydrocarbon matrix.3.1.3 total ion chromatogram(TIC),nmass spectrometercomputer output representing either the summed intensities ofall scanned ion currents or a sample of the current in the ionbeam for each spectrum scan plotted against the correspondingspectrum number.3.1.4 wall coated open tubular(WCOT),na type ofcapillary column prepared by coating or bonding the insidewall of the capillary with a thin film of stationary phase.4.Summary of Test Method4.1 A suitable internal standard,ethylbenzene d-10 is addedto the sample,which is then introduced into a gas chromato-graph equipped with two columns configured with a Deansswitching system between the two columns.The sample firstpasses through the polydimethylsiloxane(WCOT)pre-columnwhich then performs a separation of the light hydrocarbonfraction and eliminates the high boiling hydrocarbon fraction tovent.The compounds of interest and internal standard aretransferred to the high resolution polydimethylsiloxane(WCOT)analytical column for chromatographic separation.An auxiliary carrier gas is used to elute higher boilinghydrocarbons from the pre-column in back flush mode in orderto prepare for the next analysis cycle.The resulting chromato-gram is then processed by mass spectral analysis based onselected or extracted ion monitoring.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products,Liquid Fuels,and Lubricants and is the direct responsibility ofSubcommittee D02.04.0M on Mass Spectroscopy.Current edition approved April 1,2013.Published May 2013.DOI:10.1520/D7845-13.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMStandards volume information,refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.Significance and Use5.1 The test method allows the quantitation of chemicalspecies at low levels in marine fuel oils and cutter stocks.Agreat many types and concentrations of chemical species arefound in marine fuel oils.Aroot cause relationship between thepresence of such species or their concentration in fuels and anyfailure modes allegedly induced by the use of these fuels hasnot been established.This method is necessary to establish testconditions required for future ISO 8217:2010 Petroleumproducts-Fuels(class F)-Specifications of marine fuel oils asdefined in section 5.5 and Annex B item(d).Additionalcompounds may be determined by using the same conditionsand by selecti