ASTM D5134-1998(2003) Standard Test Method for Detailed Analysis of Petroleum Naphthas through n-Nonane by Capillary Gas Chromatography《用毛细管气相色谱法详细分析石脑油穿透n壬烷的标准试验方法》.pdf
《ASTM D5134-1998(2003) Standard Test Method for Detailed Analysis of Petroleum Naphthas through n-Nonane by Capillary Gas Chromatography《用毛细管气相色谱法详细分析石脑油穿透n壬烷的标准试验方法》.pdf》由会员分享,可在线阅读,更多相关《ASTM D5134-1998(2003) Standard Test Method for Detailed Analysis of Petroleum Naphthas through n-Nonane by Capillary Gas Chromatography《用毛细管气相色谱法详细分析石脑油穿透n壬烷的标准试验方法》.pdf(11页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: D 5134 98 (Reapproved 2003)An American National StandardStandard Test Method forDetailed Analysis of Petroleum Naphthas through n-Nonaneby Capillary Gas Chromatography1This standard is issued under the fixed designation D 5134; the number immediately following the designation indicates
2、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 (e) indicates an editorial change since the last revision or reapproval.INTRODUCTIONDespite the many advances in capillary gas chro
3、matography 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 theendless choices of phase thickness, column internal
4、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 example, can change resolution or elution order of
5、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 this test method to ensure consistent elution
6、order and resolution andreproducible retention times. Strict adherence to the specified conditions is essential to the successfulapplication of this test method.1. Scope1.1 This test method covers the determination of hydrocar-bon components of petroleum naphthas as enumerated in Table1. Components
7、eluting after n-nonane (bp 150.8C) are deter-mined as a single group.1.2 This test method is applicable to olefin-free (0.015 C/gMinimum detectability 5 3 1012g carbon/secondLinearity 1076.2 Sample Introduction SystemManual or automatic liq-uid syringe sample injection to the splitting injector may
8、beemployed. Devices capable of 0.2 L to 1.0 L injections aresuitable. It should be noted that inadequate splitter design orpoor injection technique, or both, can result in sample frac-tionation. Operating conditions which preclude fractionationshould be determined in accordance with Section 11.6.3 E
9、lectronic Data Acquisition SystemAny data acquisi-tion and integration device used for quantitation of theseanalyses must meet or exceed these minimum requirements:6.3.1 Capacity for at least 250 peaks/analysis.6.3.2 Normalized area percent calculation with responsefactors.6.3.3 Identification of in
10、dividual components by retentiontime.6.3.4 Noise and spike rejection capability.6.3.5 Sampling rates for fast (1 s) peaks.6.3.6 Positive and negative sloping baseline correction.6.3.7 Peak detection sensitivity for narrow and broad peaks.6.3.8 Perpendicular drop and tangent skimming as needed.6.4 Ca
11、pillary ColumnThis test method utilizes a 50-m(0.21-mm inside diameter) fused silica capillary column4withbonded (cross-linked) methyl silicone phase and a film thick-ness (df) of 0.5 m. Other columns with these nominaldimensions may be suitable. However, all columns must meetthe criteria set out in
12、 Section 10 for efficiency, resolution, andpolarity.7. Reagents and Materials7.1 Carrier Gas, helium, 99.99 % pure. (WarningCompressed gas under high pressure.)7.2 Fuel Gas, hydrogen, 99.9 % pure. (WarningExtremely flammable gas under pressure.)7.3 Make-up Gas, helium or nitrogen, 99.99 % pure.(Warn
13、ingCompressed gases under higher pressure.)7.4 n-Heptane, 99+ mol %. (WarningFlammable. Harm-ful if inhaled.)7.5 Methane(WarningExtremely flammable gas.)7.6 2-Methylheptane, 99+ mol %. (WarningFlammable.Harmful if inhaled.)7.7 4-Methylheptane, 99+ mol %. (WarningFlammable.Harmful if inhaled.)7.8 2-M
14、ethylpentane, 99+ mol %. (WarningExtremelyflammable. Harmful if inhaled.)7.9 n-Octane, 99+ mol %. (WarningFlammable. Harm-ful if inhaled.)7.10 Toluene, 99+ mol %. (WarningFlammable. Vaporharmful.)7.11 2,3,3-Trimethylpentane, 99+ mol %. (WarningExtremely flammable. Harmful if inhaled.)7.12 Column Eva
15、luation Mixture, a qualitative syntheticmixture of pure liquid hydrocarbons with the following ap-proximate composition: 0.5 % toluene, 1 % n-heptane, 1 %2,3,3-trimethylpentane, 1 % 2-methylheptane, 1 %4-methylheptane, 1 % n-octane in 2-methylpentane solvent.7.13 Reference Alkylate,5actual refinery
16、alkylation productused to prepare Fig. 1. (WarningExtremely flammable.Harmful if inhaled.)7.14 Reference Naphtha,5actual refinery stream used toprepare Fig. 2. (WarningExtremely flammable. Harmful ifinhaled.)7.15 Reference Reformate,5actual refinery reformer prod-uct used to prepare Fig. 3. (Warning
17、Extremely flammable.Harmful if inhaled.)8. Sampling8.1 Hydrocarbon liquids (including naphthas) with Reidvapor pressures of 110 kPa (16 psi) or less may be sampledeither into a floating piston cylinder or into an open container.8.1.1 Cylinder SamplingRefer to Test Method D 3700 forinstructions on tr
18、ansferring a representative sample of a hydro-carbon fluid from a source into a floating piston cylinder. Addinert gas to the ballast side of the floating piston cylinder toachieve a pressure of 350 kPa (45 psi) above the vapor pressureof the sample.8.1.2 Open Container SamplingRefer to Practice D 4
19、057for instructions on manual sampling from bulk storage intoopen containers. Stopper container immediately after drawingsample.8.2 Preserve the sample by cooling to approximately 4Cand by maintaining that temperature until immediately prior toanalysis.8.3 Transfer an aliquot of the cooled sample in
20、to a pre-cooled septum vial, then seal appropriately. Obtain the testspecimen for analysis directly from the sealed septum vial, foreither manual or automatic syringe injection.9. Preparation of Apparatus9.1 Install and condition column as per manufacturers orsuppliers instructions. After conditioni
21、ng, attach column out-let to flame ionization detector inlet and check for leaksthroughout the system. If leaks are found, tighten or replacefittings before proceeding.9.2 Calibrate the gas chromatograph column oven tempera-ture sensors using an independent, electronic temperaturemeasuring device su
22、ch as a thermocouple or platinum resis-tance temperature detector.9.2.1 Place the independent temperature measuring probe inthe oven in the region occupied by the column. Do not allowsensor to touch the walls of the oven.4The sole source of supply of the columns (designated HP-PONA) known to thecomm
23、ittee at this time is Hewlett-Packard Company, Avondale, PA. If you are awareof alternative suppliers, please provide this information to ASTM InternationalHeadquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee,1which you may attend.5These q
24、ualitative reference samples are available from Supelco, Inc., Belle-fonte, PA.D 5134 98 (2003)49.2.2 Set the oven temperature to 35C and allow oven toequilibrate for at least 15 min, then observe the temperaturereading.9.2.3 If the reading of the independent temperature sensor ismore than 0.5C diff
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