1、Designation: D5134 98 (Reapproved 2008)1D5134 13Standard Test Method forDetailed Analysis of Petroleum Naphthas through n-Nonaneby Capillary Gas Chromatography1This standard is issued under the fixed designation D5134; the number immediately following the designation indicates the year oforiginal ad
2、option 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 NOTEUpdated sole source of supply footnotes editorially in May 2008.INTRODUCTION
3、Despite the many advances in capillary gas chromatography instrumentation and the remarkableresolution achievable, it has proven difficult to standardize a test method for the analysis of a mixtureas complex as petroleum naphtha. Because of the proliferation of numerous, similar columns and theendle
4、ss choices of phase thickness, column internal diameter, length, etc., as well as instrumentoperating parameters, many laboratories use similar but not identical methods for the capillary GCanalysis of petroleum naphthas. Even minute differences in column polarity or column oventemperature, for exam
5、ple, can change resolution or elution order of components and make theiridentification an individual interpretive process rather than the desirable, objective application ofstandard retention data. To avoid this, stringent column specifications and temperature and flowconditions have been adopted in
6、 this test method to ensure consistent elution order and resolution andreproducible retention times. Strict adherence to the specified conditions is essential to the successfulapplication of this test method.1. Scope Scope*1.1 This detailed hydrocarbon analysis (DHA) test method covers the determina
7、tion of hydrocarbon components paraffins,naphthenes, and monoaromatics (PNA) of petroleum naphthas as enumerated in Table 1. Components eluting after n-nonane (bp150.8C)150.8 C) are determined as a single group.1.2 This test method is applicable to olefin-free (C7.1.5 Detailed hydrocarbon components
8、 in olefin containing samples may be determined by DHA Test Methods D6729, D6730,or D6733.1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.7 This standard does not purport to address all of the safety concerns, if any, as
9、sociated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. Specific warning statements are given in Section 7.1 This test method is under the jurisdiction of A
10、STM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.04.0L on Gas Chromatography Methods.Current edition approved May 1, 2008Dec. 1, 2013. Published September 2008January 2014. Originally approved in 1990. Last previous ed
11、ition approved in 20032008as D513498(2003).D5134 98 (2008)1. DOI: 10.1520/D5134-98R08E01.10.1520/D5134-13.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be tech
12、nically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this
13、 standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1TABLE 1 Typical Retention Characteristics of Naphtha ComponentsNOTE 1The abbreviations N and P refer to unidentified naphthenes and paraffins respectively.Compound Retention Tim
14、e, min Adjusted RetentionTime, min Kovats RetentionIndex 35C35 C Linear Retention IndexMethane 3.57 0.00 100.0 .Ethane 3.65 0.08 200.0 .Propane 3.84 0.27 300.0 .Isobutane 4.14 0.57 367.3 .n-Butane 4.39 0.82 400.0 .2,2-Dimethylpropane 4.53 0.96 415.5 .Isopentane 5.33 1.76 475.0 .n-Pentane 5.84 2.27 5
15、00.0 .2,2-Dimethylbutane 6.81 3.24 536.2 .Cyclopentane 7.83 4.26 564.1 .2,3-Dimethylbutane 7.89 4.32 565.5 .2-Methylpentane 8.06 4.49 569.5 .3-Methylpentane 8.72 5.15 583.4 .n-Hexane 9.63 6.06 600.0 .2,2-Dimethylpentane 11.22 7.65 624.2 .Methylcyclopentane 11.39 7.82 626.5 .2,4-Dimethylpentane 11.68
16、 8.11 630.3 .2,2,3-Trimethylbutane 12.09 8.52 635.4 .Benzene 13.29 9.72 649.1 .3,3-dimethylpentane 13.84 10.27 654.8 .Cyclohexane 14.19 10.62 658.3 .2-Methylhexane 15.20 11.63 667.8 .2,3-Dimethylpentane 15.35 11.78 669.1 .1,1-Dimethylcyclopentane 15.61 12.04 671.4 .3-Methylhexane 16.18 12.61 676.2 .
17、cis-1,3-Dimethylcyclopentane 16.88 13.31 681.8 .trans-1,3-Dimethylcyclopentane 17.22 13.65 684.4 .3-Ethylpentane 17.44 13.87 686.1 .trans-1,2-Dimethylcyclopentane 17.57 14.00 687.0 .2,2,4-Trimethylpentane 17.80 14.23 688.7 .n-Heptane 19.43 15.86 700.0 .Methylcyclohexane + cis-1,2-Dimethylcyclopentan
18、e 22.53 18.96 718.6A .1,1,3-Trimethylcyclopentane + 2,2-Dimethylhexane 23.05 19.48 721.4A .Ethylcyclopentane 24.59 21.02 729.3A .2,5-Dimethylhexane + 2,2,3-Trimethylpentane 25.12 21.55 731.9A .2,4-Dimethylhexane 25.47 21.90 733.5A .1,trans-2,cis-4-Trimethylcyclopentane 26.43 22.86 738.0A .3,3-Dimeth
19、ylhexane 26.79 23.22 739.6A .1,trans-2,cis-3-Trimethylcyclopentane 28.01 24.44 744.9A .2,3,4-Trimethylpentane 28.70 25.13 747.8A .Toluene + 2,3,3-Trimethylpentane 29.49 25.92 751.1A 730.2B1,1,2-Trimethylcyclopentane 31.21 27.64 . 741.7B2,3-Dimethylhexane 31.49 27.92 . 743.6B2-Methyl-3-ethylpentane 3
20、1.69 28.12 . 744.9A2-Methylheptane 33.06 29.49 . 754.1B4-Methylheptane + 3-Methyl-3-ethylpentane 33.34 29.77 . 756.0B3,4-Dimethylhexane 33.49 29.92 . 757.0B1,cis-2,trans-4-Trimethylcyclopentane + 1,cis-2,cis-4-Trimethylcyclopentane 33.73 30.16 . 758.6Bcis-1,3-Dimethylcyclohexane 34.45 30.88 . 763.4B
21、3-Methylheptane + 1,cis-2,trans-3-Trimethylcyclopentane 34.64 31.07 . 764.7B3-Ethylhexane + trans-1,4-Dimethylcyclohexane 34.83 31.26 . 766.0B1,1-Dimethylcyclohexane 35.81 32.24 . 772.5B2,2,5-Trimethylhexane + trans-1,3-Ethylmethylcyclopentane 36.75 33.18 . 778.8Bcis-1,3-Ethylmethylcyclopentane 37.1
22、4 33.57 . 781.4Btrans-1,2-Ethylmethylcyclopentane 37.39 33.82 . 783.1B2,2,4-Trimethylhexane + 1,1-Ethylmethylcyclopentane 37.68 34.11 . 785.1Btrans-1,2-Dimethylcylohexane 38.14 34.57 . 788.1B1,cis-2,cis-3-Trimethylcyclopentane 39.21 35.64 . 795.3Btrans-1,3-Dimethylcyclohexane + cis-1,4-Dimethylcyclo
23、hexane 39.54 35.97 . 797.5n-Octane 39.91 36.34 . 800.0Isopropylcyclopentane + 2,4,4-Trimethylhexane 40.76 37.19 . 805.7Unidentified C9-Naphthene 40.88 37.31 . 806.5Unidentified C8-Naphthene 41.52 37.95 . 810.8Unidentified C9-Naphthene 41.88 38.31 . 813.2cis-1,2-Ethylmethylcyclopentane + 2,3,5-Trimet
24、hylhexane 42.55 38.98 . 817.72,2-Dimethylheptane 43.20 39.63 . 822.0cis-1,2-Dimethylcyclohexane 43.43 39.86 . 823.62,2,3-Trimethylhexane + 9N 43.76 40.19 . 825.82,4-Dimethylheptane 43.88 40.31 . 826.64,4-Dimethylheptane + 9N 44.09 40.52 . 828.0Ethylcyclohexane + n-Propylcyclopentane 44.36 40.79 . 82
25、9.82-Methyl- 4-Ethylhexane 44.74 41.17 . 832.4D5134 1322. Referenced Documents2.1 ASTM Standards:2D1319 Test Method for Hydrocarbon Types in Liquid Petroleum Products by Fluorescent Indicator AdsorptionD3700 Practice for Obtaining LPG Samples Using a Floating Piston CylinderD3710 Test Method for Boi
26、ling Range Distribution of Gasoline and Gasoline Fractions by Gas ChromatographyD4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD5443 Test Method for Paraffin, Naphthene, andAromatic Hydrocarbon TypeAnalysis in Petroleum Distillates Through 200Cby Multi-Dimensional Gas Chromato
27、graphyD6839 Test Method for Hydrocarbon Types, Oxygenated Compounds, and Benzene in Spark Ignition Engine Fuels by GasChromatographyD6729 Test Method for Determination of Individual Components in Spark Ignition Engine Fuels by 100 Metre Capillary HighResolution Gas ChromatographyD6730 Test Method fo
28、r Determination of Individual Components in Spark Ignition Engine Fuels by 100Metre Capillary (withPrecolumn) High-Resolution Gas ChromatographyD6733 Test Method for Determination of Individual Components in Spark Ignition Engine Fuels by 50-Metre Capillary HighResolution Gas ChromatographyD7096 Tes
29、t Method for Determination of the Boiling Range Distribution of Gasoline by Wide-Bore Capillary GasChromatography2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the
30、standards Document Summary page on the ASTM website.TABLE 1 ContinuedCompound Retention Time, min Adjusted RetentionTime, min Kovats RetentionIndex 35C35 C Linear Retention Index2,6-Dimethylheptane + 9N 44.95 41.38 . 833.81,1,3-Trimethylcyclohexane 45.21 41.64 . 835.5Unidentified C9-Naphthene 45.56
31、41.99 . 837.82,5-Dimethylheptane + 9P 45.92 42.35 . 840.33,5-Dimethylheptane + 3,3-Dimethylheptane + N 46.09 42.52 . 841.4Unidentified C9-Naphthene 46.31 42.74 . 842.9Unidentified C9-Naphthene 46.55 42.98 . 844.5Ethyl Benzene 47.15 43.58 . 848.5Unidentified C9-Naphthene 47.37 43.80 . 850.0Unidentifi
32、ed Naphthene + 2,3,4-Trimethylhexane 47.53 43.96 . 851.0Unidentified Naphthenes 47.78 44.21 . 852.7Unidentified Naphthene + Paraffin 48.13 44.56 . 855.1m-Xylene 48.49 44.92 . 857.5p-Xylene 48.63 45.06 . 858.42,3-Dimethylheptane 48.93 45.36 . 860.43,4-DimethylheptaneC + N 49.10 45.53 . 861.63,4-Dimet
33、hylheptaneC 49.29 45.72 . 862.8Unidentified Naphthene 49.41 45.84 . 863.64-Ethylheptane + N 49.65 46.08 . 865.24-Methyloctane 50.10 46.53 . 868.32-Methyloctane 50.26 46.69 . 869.3Unidentified Naphthene 50.41 46.84 . 870.3Unidentified Naphthene 50.73 47.16 . 872.53-Ethylheptane + N 50.96 47.39 . 874.
34、03-Methyloctane 51.15 47.58 . 875.3Unidentified Naphthene 51.35 47.78 . 876.6o-Xylene + 1,1,2-Trimethylcyclohexane 51.54 47.97 . 877.9Unidentified Naphthene + 2,4,6-Trimethylheptane 51.74 48.17 . 879.2Unidentified Naphthene 52.12 48.55 . 881.8Unidentified Paraffin 52.24 48.67 . 882.6Unidentified Nap
35、hthenes 52.56 48.99 . 884.7Unidentified Naphthene 52.85 49.28 . 886.7Unidentified Naphthene + Paraffin 53.06 49.49 . 888.1Unidentified Naphthene 53.26 49.69 . 889.4Unidentified Naphthene 53.46 49.89 . 890.8Unidentified Naphthene 54.02 50.45 . 894.5Unidentified Naphthene 54.40 50.83 . 897.1n-Nonane 5
36、4.84 51.27 . 900.0Unidentified Naphthene 54.98 51.41 . 900.9A ExtrapolatedExtrapolated from n-C6 and n-C7. See A1.1.3.B ExtrapolatedExtrapolated from n-C8 and n-C9. See A1.2.3.C Stereoisomers. Stereoisomers.D5134 1333. Summary of Test Method3.1 A representative sample of the naphtha is introduced in
37、to a gas chromatograph equipped with a methyl silicone bondedphase fused silica capillary column. Helium carrier gas transports the vaporized sample through the column in which thecomponents are separated. Components are sensed by a flame ionization detector as they elute from the column.The detecto
38、r signalis processed by an electronic data acquisition system or integrating computer. Each eluting peak is identified by comparing itsretention index to a table of retention indices and by visual matching with a standard chromatogram. The table of retention indiceshas been established by running re
39、ference compounds under identical conditions or by gas chromatographicmass spectrometric(GC/MS) analysis of reference samples under the same conditions, or both.3.2 The mass concentration of each component is determined by area normalization with response factors. Peaks eluting aftern-nonane are sum
40、med and reported as C10+.4. Significance and Use4.1 A knowledge of the hydrocarbon components comprising a petroleum naphtha, reformate, or alkylate is useful in valuationof crude oils, in alkylation and reforming process control, in product quality assessment, and for regulatory purposes. Detailedh
41、ydrocarbon composition is also used as input in the mathematical modeling of refinery processes.4.2 Separation of naphtha components by the procedure described in this test method can result in some peaks that representcoeluting compounds. This test method cannot attribute relative concentrations to
42、 the coelutants. In the absence of supportinginformation, use of the results of this test method for purposes which require such attribution is not recommended.5. Interferences5.1 If present, olefinic hydrocarbons with boiling points less than 150C150 C will be separated and detected along with thes
43、aturates and aromatics. Some of the olefins will coelute with saturates or aromatics and give erroneously high concentrations forthose components. Some coelutions of PNA components above C7 may occur and results may not be completely accurate. TestMethod D5443 may be used for carbon number distribut
44、ion above C7 to verify results from this test method.5.2 Alcohols, ethers, and other organic compounds of similar volatility can also interfere by coeluting with saturate or aromatichydrocarbons thereby causing erroneously high values to be determined.6. Apparatus6.1 lnstrumentationInstrumentationA
45、gas chromatograph capable of column oven temperature programming from35C35 C to 200C200 C in 1C/min1 C/min increments is required. A heated flash vaporizing injector designed to provide alinear sample split injection (for example, 200:1) is also required for proper sample introduction.The associated
46、 carrier gas controlsmust be of adequate precision to provide reproducible column flows and split ratios in order to maintain analytical integrity. Ahydrogen flame ionization detector designed for optimum response with capillary columns (with the required gas controls andelectronics) must meet or ex
47、ceed the following specifications:Operating temperature 100C to 300COperating temperature 100 C to 300 CSensitivity 0.015 C/gMinimum detectability 5 1012 g carbon/secondLinearity 1076.2 Sample Introduction System SystemManual or automatic liquid syringe sample injection to the splitting injector may
48、 beemployed. Devices capable of 0.2 L to 1.0 L injections are suitable. It should be noted that inadequate splitter design or poorinjection technique, or both, can result in sample fractionation. Operating conditions which preclude fractionation should bedetermined in accordance with Section 11.6.3
49、Electronic Data Acquisition SystemAny data acquisition and integration device used for quantitation of these analysesmust meet or exceed these minimum requirements:6.3.1 Capacity for at least 250 peaks/analysis.6.3.2 Normalized area percent calculation with response factors.6.3.3 Identification of individual components by retention time.6.3.4 Noise and spike rejection capability.6.3.5 Sampling rates for fast (carbon number C7.(2) Added references to DHA and other pertinent test methods.ASTM International takes no position respecting the v
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