1、Designation: D7875 14Standard Test Method forDetermination of Butanol and Acetone Content of Butanolfor Blending with Gasoline by Gas Chromatography1This standard is issued under the fixed designation D7875; the number immediately following the designation indicates the year oforiginal adoption or,
2、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 determination of the butanolcontent of butanol for bl
3、ending with gasoline by gas chroma-tography.1.2 Butanol is determined from 95 % to 99.9 % by mass,acetone is determined from 0.02 % to 1.5 % by mass, ethanolis determined from 0.02 % to 1.5 % by mass, and methanol isdetermined from 0.02 % to 1.5 % by mass. Equations used toconvert these individual c
4、omponents from mass percent tovolume percent are provided.1.3 This test method identifies and quantifies acetone,ethanol, and methanol, but does not purport to identify allindividual components that may be present in butanol forgasoline blending.1.4 Water cannot be determined by this test method and
5、shall be measured by a procedure such as Test Method D1364and the result used to correct the chromatographic values.1.5 This test method is inappropriate for impurities that boilat temperatures higher than 225 C or for impurities that causepoor or no response in a flame ionization detector, such asw
6、ater.1.6 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.7 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
7、 appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1298 Test Method for Density, Relative Density, or APIGravity of Crude Petroleum and Liquid Petroleum Prod-ucts by Hydrometer MethodD1364 Test
8、 Method for Water in Volatile Solvents (KarlFischer Reagent Titration Method)D4052 Test Method for Density, Relative Density, and APIGravity of Liquids by Digital Density MeterD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4307 Practice for Preparation of Liquid Blends for Use
9、 asAnalytical StandardsD4626 Practice for Calculation of Gas ChromatographicResponse FactorsD4806 Specification for Denatured Fuel Ethanol for Blend-ing with Gasolines for Use as Automotive Spark-IgnitionEngine FuelD6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniq
10、ues to Evaluate AnalyticalMeasurement System PerformanceD6300 Practice for Determination of Precision and BiasData for Use in Test Methods for Petroleum Products andLubricantsD7862 Specification for Butanol for Blending with Gasolinefor Use as Automotive Spark-Ignition Engine FuelE355 Practice for G
11、as Chromatography Terms and Relation-shipsE594 Practice for Testing Flame Ionization Detectors Usedin Gas or Supercritical Fluid ChromatographyE1064 Test Method for Water in Organic Liquids by Coulo-metric Karl Fischer Titration3. Terminology3.1 DefinitionsThis test method makes reference to manycom
12、mon gas chromatographic procedures, terms, and relation-ships. Detailed definitions can be found in Practices E355 andE594.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.04.0L on
13、 Gas Chromatography Methods.Current edition approved July 1, 2014. Published September 2014. DOI:10.1520/D7875-14.2For 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 th
14、e standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.1.1 butanol, nfor the purposes of this method, butanol orbutyl alcohol refers to one of three structural isomers ofbutanol1-butanol
15、, 2-butanol, and 2-methyl-1-propanol. Thistest method has not been evaluated for use with the butanolisomer 2-methyl-2-propanol.4. Summary of Test Method4.1 A representative aliquot of the butanol sample is intro-duced into a gas chromatograph equipped with a polydimeth-ylsiloxane bonded phase capil
16、lary column. Helium carrier gastransports the vaporized aliquot through the column where thecomponents are separated by the chromatographic process.Components are sensed by a flame ionization detector as theyelute from the column. The detector signal is processed by anelectronic data acquisition sys
17、tem. The butanol, acetone,ethanol, and methanol components are identified by comparingtheir retention times to the ones identified by analyzingstandards under identical conditions. The concentrations of allcomponents are determined in mass percent area by normal-ization of the peak areas.5. Signific
18、ance and Use5.1 Butanol is being approved for blending with gasoline inaccordance with Specification D7862. This test method pro-vides a method of determining the percentage of butanol(purity) of the butanol for blending with gasoline.6. Apparatus6.1 Gas Chromatograph, capable of operating at the co
19、ndi-tions listed in Table 1. A heated flash vaporizing injectordesigned to provide a linear sample split injection (forexample, 200:1) is required for proper sample introduction.Carrier gas controls shall be of adequate precision to providereproducible column flows and split ratios in order to maint
20、ainanalytical integrity. Pressure control devices and gauges shallbe designed to attain the linear velocity required in the columnused. A hydrogen flame ionization detector with associated gascontrols and electronics, designed for optimum response withopen tubular columns, is required.6.2 Sample Int
21、roductionManual or automatic liquid sy-ringe sample injection to the splitting injector is employed.Devices capable of 1.0 L injections are suitable. It should benoted that inadequate splitter design, poor injection technique,and overloading the column can result in poor resolution.Avoid overloading
22、, particularly of the butanol peak(s), andeliminate this condition during analysis.6.3 ColumnThis test method utilizes a fused silica opentubular column with non-polar polydimethylsiloxane bonded(cross-linked) phase internal coating.Any column with equiva-lent or better chromatographic efficiency an
23、d selectivity to thatdescribed in 6.3.1 can be used.6.3.1 Open tubular column with a non-polar polydimethyl-siloxane bonded (cross-linked) phase internal coating; a 150 mlong by 0.25 mm internal diameter column with a 1.0 m filmthickness has been found to be suitable.6.4 Electronic Data Acquisition
24、SystemAny data acquisi-tion and integration device used for quantification of theseanalyses must meet or exceed these minimum requirements:6.4.1 Capacity for at least 80 peaks/analysis,6.4.2 Normalized percent calculation based on peak areaand using response factors,6.4.3 Identification of individua
25、l components based on re-tention time,6.4.4 Noise and spike rejection capability,6.4.5 Sampling rate for narrow (96 %butanol).13.1.2 Prepare standard(s) in sufficient volume to allow fora minimum of 30 quality control measurements to be made onone batch of material. Properly package and store the qu
26、alitycontrol samples to ensure that all analyses of quality controlsamples from a given lot are performed on essentially identicalmaterial. Use of the Q-procedure in Practice D6299 is recom-mended when switching between batches of control sample.14. Report14.1 Report the purity of butanol as the sum
27、 of the amountsof 1-butanol, 2-butanol, and 2-methyl-1-propanol to the nearest0.01 % by mass using Eq 3 or nearest 0.01 % by volume usingEq 4. Report individually acetone, ethanol, and methanol to thenearest 0.01 % by mass.15. Precision and Bias15.1 The precision of this test method was determined b
28、ystatistical examination of limited laboratory results. The preci-sion data are provisional, and further data are to be developedin an interlaboratory cooperative test program before thefive-year reapproval (2018) required by the society.15.2 PrecisionThe precision of this test method as deter-mined
29、 by the statistical examination of gas chromatographictest results from a single laboratory using Practice D6300 forthe design and analysis of the data as follows:15.2.1 RepeatabilityThe difference between successiveresults obtained by the same operator with the same apparatusunder constant operatin
30、g conditions on identical test materialswould, in the long run, in the normal and correct operation ofthe test method exceed the following values only in one case intwenty.Butanol RepeatabilityAComponent Range,Mass PercentRepeatability,Mass percent2-methyl-1-propanol 95 to 99.9 0.2051-butanol 95 to
31、99.9 0.3502-butanol 95 to 99.9 0.366acetone 0.02 to 1.5 0.000185*(X)1/2methanol 0.02 to 1.5 0.000199*(X)1/2ethanol 0.02 to 1.5 0.000202(X)1/2Awhere X is the mass percent.NOTE 2The data below shows the repeatability for butanols andseveral acetone values obtained using the formula given in 15.2.1.But
32、anol Repeatabilityamount (mass percent r2-Methyl-1-propanol 95 to 99.9 0.2051-Butanol 95 to 99.9 0.3502-Butanol 95 to 99.9 0.366Acetone in 2-Methyl-1-propanol 1.50 0.000226Acetone in 2-Methyl-1-propanol 1.00 0.000194Acetone in 2-Methyl-1-propanol 0.70 0.000154Acetone in 2-Methyl-1-propanol 0.25 0.00
33、0092Acetone in 2-Methyl-1-propanol 0.10 0.000058Acetone in 2-Methyl-1-propanol 0.02 0.000026Acetone in 1-Butanol 1.50 0.000378Acetone in 1-Butanol 1.00 0.000323Acetone in 1-Butanol 0.70 0.000258Acetone in 1-Butanol 0.25 0.000154Acetone in 1-Butanol 0.10 0.000097Acetone in 1-Butanol 0.02 0.000044Acet
34、one in 2-Butanol 1.50 0.000411Acetone in 2-Butanol 1.00 0.000352Acetone in 2-Butanol 0.70 0.000281Acetone in 2-Butanol 0.25 0.000168Acetone in 2-Butanol 0.10 0.000106Acetone in 2-Butanol 0.02 0.000047NOTE 3The data below shows the repeatability for butanols andseveral ethanol values obtained using t
35、he formula given in 15.2.1.Butanol Repeatabilityamount (mass percent r2-Methyl-1-propanol 95 to 99.9 0.2051-Butanol 95 to 99.9 0.3502-Butanol 95 to 99.9 0.366Ethanol in 2-Methyl-1-propanol 1.50 0.000247Ethanol in 2-Methyl-1-propanol 1.00 0.000212Ethanol in 2-Methyl-1-propanol 0.70 0.000169Ethanol in
36、 2-Methyl-1-propanol 0.25 0.000101Ethanol in 2-Methyl-1-propanol 0.10 0.000064Ethanol in 2-Methyl-1-propanol 0.02 0.000029Ethanol in 1-Butanol 1.50 0.000413Ethanol in 1-Butanol 1.00 0.000354Ethanol in 1-Butanol 0.70 0.000282Ethanol in 1-Butanol 0.25 0.000169Ethanol in 1-Butanol 0.10 0.000107Ethanol
37、in 1-Butanol 0.02 0.000048Ethanol in 2-Butanol 1.50 0.000437Ethanol in 2-Butanol 1.00 0.000375Ethanol in 2-Butanol 0.70 0.000299Ethanol in 2-Butanol 0.25 0.000179Ethanol in 2-Butanol 0.10 0.000113Ethanol in 2-Butanol 0.02 0.000051NOTE 4The data below shows the repeatability for butanols andseveral m
38、ethanol values obtained using the formula given in 15.2.1.D7875 146Butanol Repeatabilityamount (masspercentr2-Methyl-1-propanol 95 to 99.9 0.2051-Butanol 95 to 99.9 0.3502-Butanol 95 to 99.9 0.366Methanol in 2-Methyl-1-propanol 1.50 0.000243Methanol in 2-Methyl-1-propanol 1.00 0.000208Methanol in 2-
39、Methyl-1-propanol 0.70 0.000166Methanol in 2-Methyl-1-propanol 0.25 0.000099Methanol in 2-Methyl-1-propanol 0.10 0.000063Methanol in 2-Methyl-1-propanol 0.02 0.000028Methanol in 1-Butanol 1.50 0.000415Methanol in 1-Butanol 1.00 0.000355Methanol in 1-Butanol 0.70 0.000284Methanol in 1-Butanol 0.25 0.
40、000169Methanol in 1-Butanol 0.10 0.000107Methanol in 1-Butanol 0.02 0.000048Butanol Repeatabilityamount (masspercentrMethanol in 2-Butanol 1.50 0.000458Methanol in 2-Butanol 1.00 0.000392Methanol in 2-Butanol 0.70 0.000313Methanol in 2-Butanol 0.25 0.000187Methanol in 2-Butanol 0.10 0.000188Methanol
41、 in 2-Butanol 0.02 0.00005315.2.2 ReproducibilityReproducibility was not deter-mined for this test method.15.2.3 BiasBias was not determined for this test method.16. Keywords16.1 acetone; bio-butanol; butanol; fuel grade butanol; gaschromatographyASTM International takes no position respecting the v
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