1、Designation: D5008 07 (Reapproved 2012)Standard Test Method forEthyl Methyl Pentanol Content and Purity Value of2-Ethylhexanol By Gas Chromatography1This standard is issued under the fixed designation D5008; 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. Scope*1.1 This test method covers the determination of ethylmethyl pentanol content and pu
3、rity value of 2-ethylhexanol.1.2 Water and acid cannot be determined by this test methodand must be determined in accordance with Test MethodsD1613 and E203 and those results used to normalize thechromatographic data.1.3 For purposes of determining conformance of an ob-served or a calculated value u
4、sing this test method to relevantspecifications, test result(s) shall be rounded off “to the nearestunit” in the last right-hand digit used in expressing thespecification limit, in accordance with the rounding-off methodof Practice E29.1.4 The values stated in SI units are to be regarded asstandard.
5、 No other units of measurement are included in thisstandard.1.5 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-b
6、ility of regulatory limitations prior to use. For a specifichazard statement, see 6.1.1.1.6 For hazard information and guidance, see the suppliersMaterial Safety Data Sheet.2. Referenced Documents2.1 ASTM Standards:2D1613 Test Method for Acidity in Volatile Solvents andChemical Intermediates Used in
7、 Paint, Varnish, Lacquer,and Related ProductsE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE203 Test Method for Water Using Volumetric Karl FischerTitration3. Summary of Test Method3.1 A representative specimen is introduced onto a capillarycolumn.
8、 The 2-ethylhexanol is separated from the ethyl methylpentanol and other impurities while the components are trans-ported through the column by an inert carrier gas. Theseparated components are measured in the effluent by a flameionization detector and the areas for the peaks are determinedby a suit
9、able integration technique. The data are interpreted byapplying component detector response factors to the peakareas, and the relative concentrations are determined by relat-ing the individual peak responses to the total peak response.Acidity and water are measured by Test Methods D1613 andE203, res
10、pectively, and the results are used to normalize thevalues obtained by gas chromatography. An internal standardprocedure is also included as an alternative calculation tech-nique. With this procedure, all impurities are determinedrelative to the internal standard and the purity value isdetermined by
11、 subtracting the sum of the impurities, water, andacid from 100.4. Significance and Use4.1 This test method is used to determine the purity valueand ethyl methyl pentanol content of 2-ethylhexanol.5. Apparatus5.1 ChromatographAny gas chromatograph designed ormodified for use with capillary or wide-b
12、ore capillary columns.The gas chromatograph should be equipped with a flameionization detector or other detector capable of operating withthese columns and capable of detecting impurities at a level of0.01 weight % with a signal to noise ratio of at least 5:1.5.2 ColumnAny column capable of resolvin
13、g2-ethylhexanol from ethyl methyl pentanol and other impuri-ties that may be present. The peaks should be resolvedquantitatively within a practical elapsed time. Columns thatmeet the requirement of this test method are listed in Table 1.Other columns may be used, provided the user establishes thata
14、column gives the required separations.1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.Current edition approved July
15、 1, 2012. Published September 2012. Originallyapproved in 1989. Last previous edition approved in 2007 as D5008 07. DOI:10.1520/D5008-07R12.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volum
16、e information, refer to the standards Document Summary page onthe ASTM website.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.3 Specimen Introduction SystemAny system
17、 capable ofintroducing a representative specimen into the gas chromato-graph may be used. A 1-L syringe has been used successfully.5.4 Computing IntegratorAny computing integrator ca-pable of accurately determining the peak areas generatedduring this analysis.5.5 Analytical BalanceThe internal stand
18、ard techniquerequires an analytical balance capable of measuring 0.1 mg.6. Reagents and Materials6.1 Carrier GasHelium, purified nitrogen, or hydrogenare suitable. The carrier gas should have a minimum purity of99.95 mol %.6.1.1 Warning: If hydrogen is used, take special safetyprecautions to ensure
19、that the chromatographic system is freefrom leaks.6.2 Detector GasesHydrogen and air are used for theflame ionization detector. If a make-up gas is used, helium ornitrogen are suitable.6.3 Standards for Calibration and Identification Standardsamples for all identifiable components present are needed
20、 foridentification by retention time, and for calibration for quanti-tative measurements. In the case of the internal standardmethod, pure (99.0 + %) 2-ethyl-1-butanol is specified as theinternal standard. Any other internal standard may be usedprovided it is not present in the sample and doesnt int
21、erferewith any other chromatographic peak with the column used.7. Calibration and Standardization7.1 IdentificationSelect the conditions of column, columntemperature and carrier-gas flow that will give the necessarycomponent resolution (see Table 1). Determine the retentiontime for each component by
22、 injecting small amounts of thecompound either separately or in mixtures.7.2 StandardizationThe area under each peak generated isconsidered a quantitative measure of the corresponding com-pound. The relative area is proportional to concentration if thedetector responds equally to all the sample comp
23、onents. Theresponse to different components is generally significantlydifferent for flame ionization detectors. This difference indetector response may be corrected by use of relative responsefactors obtained by injecting and measuring the response ofknown blends. Using pure materials, prepare a cal
24、ibrationmixture with each component present in the appropriateamount. If an internal standard calculation technique is used,include the internal standard in this calibration mixture. If purecomponents are not available and interfering components arepresent, then appropriate adjustments must be made
25、in calcu-lating the weights of the components present.7.2.1 Chromatographic ConditionsUsing a suitablemethod selected from Table 1, analyze a representative speci-men of the calibration mixture.7.2.2 If a computing integrator is used, follow the manufac-turers instruction manual to calculate relativ
26、e response factors.If manual calculations are used, calculate relative responsefactors for each component as follows:TABLE 1 Conditions and Retention TimesCase I Case II Case IIIColumn:Material fused silica fused silica fused silicaLength, m 10 10 30Inside diameter, mm 0.53 0.53 0.32Liquid phase imm
27、obilized polydimethylsiloxane immobilized polydimethylsiloxane immobilized polyethylene glycolFilm thickness, m 5 5 0.25Injection system: direct flash vaporization direct flash vaporization splitInjection specimen size, L 0.1 0.1 1Temperatures:Column temperature, C (isothermal) 85 85 120Injection po
28、rt temperature, C 200 200 220Detector temperature, C 200 200 220Gases:Carrier gas helium helium heliumCarrier gas flow rate, mL/min 4 4 0.6Carrier gas velocity, cm/s 30 30 20Hydrogen flow rate (detector), mL/min30 30 30Air flow rate (detector), mL/min 300 300 300Make-up gas none none heliumMake-up f
29、low rate (detector), mL/min none none 30Injection split ratioAA50:1Calculation technique: normalization internal standard normalizationTypical retention time, min:2-ethyl-2-butanol (internal standard)A2.24AEthyl methyl pentanol 5.75 5.75 5.742-ethylhexanol 7.76 7.76 7.24ANot applicable.D5008 07 (201
30、2)2R 5 A 3 B!/C 3 D! (1)where:R = response factor for component of interest,A = peak area of reference component,B = weight of component of interest in calibration mixture,g,C = peak area for component of interest in calibrationmixture, andD = weight of reference component in calibration mixture, g.
31、NOTE 1If a normalization calculation technique is used,2-ethylhexanol will be the reference component. If an internal standardcalculation technique is used, the internal standard will be the referencecomponent.7.2.3 The calibration factor generated for ethyl methylpentanol can be used to calculate t
32、he concentration of anyunknowns present.8. Procedure8.1 Normalization Technique:8.1.1 Introduce a representative specimen into the chro-matograph.8.1.2 Using the same conditions as for calibration andstandardization, determine the areas for all peaks.8.2 Internal Standard Technique:8.2.1 Weigh 0.1 g
33、 of internal standard into a vial. Record theweight to the nearest 0.1 mg.8.2.2 Into the same vial, weigh 20.0 g of a representativespecimen. Record the weight to the nearest 0.1 mg. Close thevial tightly and mix well.8.2.3 Introduce a representative specimen of the mixture in8.2.2 into the gas chro
34、matograph.8.2.4 Using the same conditions as for calibration andstandardization, determine the areas for all peaks.9. Calculation9.1 Normalization Technique:9.1.1 If a computing integrator is used, follow the manufac-turers instruction manual to compute the percent of eachcomponent of interest.9.1.2
35、 If manual calculations are made, apply the appropriatedetector response factor to each peak to obtain the correctedpeak response. Calculate the weight percent, W, of eachcomponent of interest as follows:W 5 E/F! 3 100 2 G! (2)where:E = corrected peak response for component of interest,F = sum of co
36、rrected peak responses for all components,andG = sum of water and acid as determined by Test MethodsD1613 and E203.9.2 Internal Standard Technique :9.2.1 If a computing integrator is used, follow the manufac-turers instruction manual to compute the percent of eachcomponent except the 2-ethylhexanol.
37、9.2.2 If manual calculations are made, apply the appropriatedetector response factor to each peak to obtain the correctedpeak response. Calculate the weight percent W of eachcomponent, except the 2-ethylhexanol, as follows:W 5 H 3 I 3100!/J 3 K! (3)where:H = corrected peak response for component of
38、interest,I = weight of internal standard added to sample, g,J = corrected peak response for internal standard, andK = weight of sample mixed with internal standard, g.9.2.3 Calculate the purity value, P, in weight percent asshown below:P 5 100 2 L (4)where:L = sum of water, acid, and the weight perc
39、ent of allcomponents except 2-ethylhexanol.10. Report10.1 Report the following information:10.1.1 The ethyl methyl pentanol content to the nearest0.001 weight % and10.1.2 The purity value to the nearest 0.01 weight %.11. Precision and Bias311.1 In an interlaboratory study of this test method in whic
40、hone operator in ten laboratories tested 2-ethylhexanol with apurity value of 99.653 and which contained 0.203 weight % ofethyl methyl pentanol, the within-laboratory standard deviationand between-laboratory standard deviation, with 9 df,respectively, were as follows:Standard Deviation, weight %With
41、inLaboratoryBetweenLaboratoryEthyl methyl pentanol2-Ethylhexanol0.0020.0060.0110.04011.1.1 Based upon these standard deviations, the followingcriteria should be used for judging the acceptability of resultsat the 95 % confidence level.11.1.2 RepeatabilityTwo results, each the mean of dupli-cates obt
42、ained by the same operator on different days, shouldbe considered suspect if they differ by more that 0.02 weight %absolute for purity values or 0.007 weight % absolute for ethylmethyl pentanol.11.1.3 ReproducibilityTwo results, each the mean of du-plicates obtained by operators in different laborat
43、ories, shouldbe considered suspect if they differ by more than 0.13 weight% absolute for purity values or 0.036 weight % absolute forethyl methyl pentanol.11.2 BiasThe bias of this test method has not beendetermined because a suitable reference standard is not avail-able.12. Keywords12.1 ethyl methy
44、l pentanol content/composition by gaschromatography; purity by gas chromatography;2-ethylhexanol3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D01-1118.D5008 07 (2012)3SUMMARY OF CHANGESCommittee D01.35 has identified the locat
45、ion of selected changes to this standard since the last issue(D5008 - 01) that may impact the use of this standard. (Approved June 1, 2007.)(1) Added reference to Practice E29 in the Scope section. (2) Added Practice E29 to list of Referenced Documents.ASTM International takes no position respecting
46、 the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standar
47、d is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International
48、 Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.Thi
49、s standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D5008 07 (2012)4
