1、Designation: D 5008 07Standard Test Method forEthyl Methyl Pentanol Content and Purity Value of2-Ethylhexanol By Gas Chromatography1This standard is issued under the fixed designation D 5008; the number immediately following the designation indicates the year oforiginal adoption or, in the case of r
2、evision, 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.1. Scope*1.1 This test method covers the determination of ethylmethyl pentanol content and purity value of 2
3、-ethylhexanol.1.2 Water and acid cannot be determined by this test methodand must be determined in accordance with Test MethodsD 1613 and E 203 and those results used to normalize thechromatographic data.1.3 For purposes of determining conformance of an ob-served or a calculated value using this tes
4、t 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. No other uni
5、ts 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-bility of regu
6、latory 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:D 1613 Test Method for Acidity in Volatile Solvents andChemical Intermediates Used in Paint, Varni
7、sh, Lacquer,and Related ProductsE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE 203 Test Method for Water Using Volumetric Karl FischerTitration3. Summary of Test Method3.1 A representative specimen is introduced onto a capillarycolumn. The 2-ethyl
8、hexanol 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 suitable integra
9、tion 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 D 1613 andE 203, respectively,
10、 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 subtracti
11、ng 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-bore capill
12、ary 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 resolving2-ethylhe
13、xanol 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 1.1This test method is under the jurisdiction of ASTM Committee D01 on Pain
14、tand Related Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.Current edition approved June 1, 2007. Published July 2007. Originally approvedin 1989. Last previous edition approved in 2001 as D 5008 01.
15、1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.Other columns may be used, provided the user establishes thata column gives the required separations.5.3 Specimen Intro
16、duction SystemAny system 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 B
17、alanceThe internal standard 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 safe
18、typrecautions to ensure 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 IdentificationStandardsamples for all identifiable compon
19、ents present are needed 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 th
20、e sample and doesnt interferewith 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 retentiontim
21、e for each component by 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
22、 to all the sample components. 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 m
23、aterials, prepare a calibrationmixture 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 ad
24、justments must be made 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 manu
25、al to calculate relative response factors.If manual calculations are used, calculate relative responsefactors for each component as follows.R 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
26、 mix-ture, g,C = peak area for component of interest in calibrationmixture, andTABLE 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 immobilized polydimethylsiloxane immobili
27、zed 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 port temperature, C 200 200 220Detector
28、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 flow rate (detector), mL/min none none
29、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.D5008072D = weight of reference component in calibr
30、ation mixture,g.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 use
31、d to calculate the 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
32、.2.1 Weigh 0.1 g 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 i
33、nto the gas chromatograph.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 o
34、f interest.9.1.2 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 of interest as follows:W 5 E/F! 3 100 2 G!(2)where:E = corrected peak response for component of interes
35、t,F = sum of corrected peak responses for all components,andG = sum of water and acid as determined by Test MethodsD 1613 and E 203.9.2 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
36、 2-ethylhexanol.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 each com-ponent, except the 2-ethylhexanol, as follows:W 5 H 3 I 3 100!/J 3 K! (3)where:H = corrected peak respons
37、e for component of 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,
38、and the weight percent 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 Bias211.1 In an interlaboratory study of this
39、test method in whichone 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, respec-tively, were as follows:Standard De
40、viation, weight %WithinLaboratoryBetweenLaboratoryEthyl 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 me
41、an of dupli-cates obtained 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
42、 in different laboratories, 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. Key
43、words12.1 ethyl methyl pentanol content/composition by gaschromatography; purity by gaschromatography;2-ethylhexanol2Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D01-1118.D5008073SUMMARY OF CHANGESCommittee D01.35 has identifi
44、ed the location of selected changes to this standard since the last issue(D 5008 - 01) that may impact the use of this standard. (Approved June 1, 2007.)(1) Added reference to Practice E29in the Scope section. (2) Added Practice E29to list of Referenced Documents.ASTM International takes no position
45、 respecting 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.T
46、his standard 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 In
47、ternational 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 show
48、n below.This 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).D5008074
