1、Designation: D3329 03 (Reapproved 2017)Standard Test Method forPurity of Methyl Isobutyl Ketone by Gas Chromatography1,2This standard is issued under the fixed designation D3329; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the
2、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.This standard has been approved for use by agencies of the U.S. Department of Defense.1. Scope1.1 This test method covers
3、the determination of the purityof methyl isobutyl ketone (MIBK) by gas chromatography andin addition provides a means for measuring certain impuritiessuch as methyl isobutyl carbinol which are of interest. Impu-rities such as water and acidity are measured by other appro-priate ASTM procedures and t
4、he results are used to normalizethe chromatographic value.1.2 The following applies to all specified limits in thisstandard; for purposes of determining conformance with thisstandard, an observed value or a calculated value shall berounded off “to the nearest unit” in the last right-hand digitused i
5、n expressing the specification limit, in accordance withthe round-off method of Practice E29.1.3 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.4 This standard does not purport to address all of thesafety concerns, if any, a
6、ssociated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.5 For specific hazard information and guidance, see thesuppliers Safety Data Sh
7、eet for the materials listed in this testmethod.1.6 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by t
8、he World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1364 Test Method for Water in Volatile Solvents (KarlFischer Reagent Titration Method)D1613 Test Method for Acidity in Volatile Solvents andChemical Intermediates Used in Paint, Varnish
9、, Lacquer,and Related ProductsD2593 Test Method for Butadiene Purity and HydrocarbonImpurities by Gas ChromatographyE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of
10、 Industrial and Spe-cialty Chemicals (Withdrawn 2009)3E260 Practice for Packed Column Gas Chromatography3. Summary of Test Method3.1 A representative specimen is introduced onto a gas-liquid partition column. Methyl isobutyl ketone is separatedfrom impurities such as acetone, 2-propanol, pentanone,
11、mesi-tyl oxide, methyl isobutyl carbinol, and several unidentifiedcompounds as the components are transported through thecolumn by an inert carrier gas. The separated components aremeasured in the effluent by a detector and recorded as achromatogram. The chromatogram is interpreted by applyingcompon
12、ent attenuation and detector response factors to thepeak areas, and the relative concentrations are determined byrelating the individual peak responses to the total peak re-sponse. Water and acidity are measured in accordance with TestMethods D1364 and D1613 and the results are used tonormalize the
13、values obtained by gas chromatography.4. Significance and Use4.1 This test method provides a measurement of commonlyfound impurities in commercially available methyl isobutylketone. The measurement of these impurities and the resultsthereof can individually or when totaled and subtracted from100 (as
14、say) be used for specification acceptance.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
15、Dec. 1, 2017. Published December 2017. Originallyapproved in 1974. Last previous edition approved in 2009 as D3329 03 (2009).DOI: 10.1520/D3329-03R17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStand
16、ards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis internati
17、onal standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committ
18、ee.15. Apparatus5.1 ChromatographAny gas liquid chromatographic in-strument having either a thermal conductivity or flame ioniza-tion detector provided the system has sufficient sensitivity andstability to obtain for 0.01 % of impurity a recorder deflectionof at least 2 mm at a signal-to-noise ratio
19、 of at least 5 to 1. Thespecimen size used in judging the sensitivity must be such thatthe column is not overloaded, which would result in peakbroadening, loss of resolution, shifting retention times andformation of leading peaks.5.2 ColumnAny column capable of resolving methylisobutyl ketone from t
20、he impurities that may be present.Possible impurities are hydrocarbons, acetone, 2-propanol,2-pentanone, 3-pentanone, mesityl oxide, mesityl oxideisomer, and methyl isobutyl carbinol. Columns that meet thisrequirement are described in Table 1. Other columns, includingcapillary columns, may be used,
21、provided the user establishesthat a column gives the required separation and the peak shapesare satisfactory for measurement so that the precision require-ments of Section 12 are met.5.3 Specimen Introduction SystemAny system capable ofintroducing a representative specimen onto the column. Mi-crolit
22、re syringes have been used successfully.5.4 RecorderA recording potentiometer with a full-scaledeflection of 5 mV or less, full-scale response time of2sorless, and sufficient sensitivity and stability to meet the require-ments of 5.1.6. Reagents and Materials6.1 Carrier GasCarrier gas appropriate to
23、 the type ofdetector used. Helium or hydrogen may be employed withthermal conductivity detectors and nitrogen, helium, or argonwith flame ionization detectors. The minimum purity of thecarrier gas used should be 99.95 mol %. (Warning Ifhydrogen is used, take special safety precautions to ensure that
24、the system is free from leaks and that the effluent is ventedproperly.)6.2 Column Materials:6.2.1 Liquid PhaseThe materials successfully used incooperative test work are listed in Table 1. (See Note 1.)NOTE 1Suppliers of liquid phases and supports can be found inResearch Report RR:D01-1042, availabl
25、e from ASTM InternationalHeadquarters.6.2.2 Solid SupportThe materials and their mesh sizessuccessfully used in cooperative work are shown in Table 1.(See Note 1.)6.2.3 Tubing MaterialCopper, stainless steel, and alumi-num have been found satisfactory for column tubing. Thetubing must be nonreactive
26、 with the substrate, sample, andcarrier gas and be of uniform internal diameter.6.3 Standards for Calibration and IdentificationStandardsamples of all components present are needed for identificationby retention time and for calibration for quantitative measure-ments.7. Preparation of Apparatus7.1 C
27、olumn PreparationThe method used to prepare thecolumn is not critical provided that the finished columnproduces the required separation (Note 2). Partitioning liquids,supports, and loading levels used successfully in cooperativework are listed in Table 1.NOTE 2A suitable method for column preparatio
28、n is described in TestMethod D2593. Additional useful information may be found in PracticeE260.TABLE 1 Columns and Conditions Used Successfully in Cooperative Work (See Note 1)Case I Case II Case III Case IV Case V Case VIColumn:Liquid phase polyethylene glycol,MW 1450polyethylene glycol,MW 540ethyl
29、ene oxide/propylene oxidecopolymerpolyethylene glycol,MW 20Mpolyethylene glycol,MW 3350polyethylene glycolLiquid phase, weight % 15 20 20 25 25 1.2 m filmSupport diatomaceous earth,acid washeddiatomaceous earth diatomaceous earth,acid washeddiatomaceous earth diatomaceous earth capillarySupport mesh
30、 size 60 to 80 60 to 80 45 to 60 60 to 80 60 to 80 N/ALength, m (ft) 6.1 (20) 5.5 (18) 6.1 (20) 3.0 (10) 3.7 (12) 10 (33)Diameter, mm (in.) 3.2 (18 ) 6.4 (14 ) 6.4 (14 ) 3.2 (18 ) 6.4 (14 ) 0.53 (0.021)Temperature, C 90 100 160 75 to 200programmed at4/min145 40 to 180 at5/minCarrier gas: helium heli
31、um helium helium helium heliumFlow rate, mL/min 30 50 60 20 80 5Typical retention time, min:Methyl isobutyl ketone 9.3 27.2 8.1 11.2 7.7 1.84Relative retention time,MIBK = 1.00:Acetone 0.42 0.39 0.52 0.42 0.39 0.362-propanol 0.66 0.57 0.65 0.56 0.592- and 3-pentanone 0.85 0.82 0.78 . . 0.79Methyl is
32、obutyl ketone 1.00 1.00 1.00 1.00 1.00 1.00-Mesityl oxide 1.45 1.41 1.27 . . .-Mesityl oxide 1.89 1.85 1.63 1.24 1.52 .Methyl isobutyl carbinol 2.11 2.07 1.48 1.42 1.95 2.24D3329 03 (2017)27.1.1 Prepacked columns conforming to requirements listedin Table 1 and in 5.2 and 6.2 may be obtained from any
33、reputable chromatography supply company.7.2 ChromatographInstall the column in the chromato-graph and establish the operating conditions required to givethe desired separation. Allow sufficient time for the instrumentto reach equilibrium as indicated by a stable recorder baseline.Control the detecto
34、r temperature so that it is constant to within1C without thermostat cycling that causes an uneven baseline.Adjust the carrier-gas flow rate to a constant value.8. Calibration and Standardization8.1 IdentificationSelect the conditions of column tem-perature and carrier gas flow that will give the nec
35、essaryresolution of the components. Determine the retention time ofeach component by injecting small amounts either separatelyor in known mixtures. Relative component retention timesalong with the typical retention time for methyl isobutyl ketoneare given in Table 1.8.2 StandardizationThe area under
36、 each peak of thechromatogram is considered a quantitative measure of thecorresponding compound. The relative area is proportional toconcentration if the detector responds equally to all the samplecomponents. When flame ionization detectors are used theresponse to different components is generally s
37、ignificantlydifferent. Differences in detector response may be corrected byuse of relative response factors obtained by injecting andmeasuring the response to pure (99 weight % minimum)components or known blends. When thermal conductivitydetectors are used for the analysis of high-purity methylisobu
38、tyl ketone, the difference between area percent andweight percent is within the precision of the test method.NOTE 3Much data on thermal conductivity and flame ionizationdetector responses may be found in the literature. Useful information isgiven by Messner, et al4and by Dietz.59. Procedure9.1 Intro
39、duce a representative specimen into the chromato-graph using a microlitre syringe. Use sufficient specimen toensure a minimum of 10 % recorder deflection for a 0.1 %concentration of impurity at the most sensitive setting of theinstrument.9.2 Using the same conditions as for component identifica-tion
40、 and standardization, record the peaks of all components atattenuation settings that provide maximum peak heights.10. Calculation10.1 Measure the area of all peaks (Note 4) and multiplyeach area by the appropriate attenuation factor to express thepeak areas on a common basis. If a flame ionization d
41、etectorwas used, apply the appropriate detector response factors tocorrect for the difference in response to the components.Calculate the weight percent composition by dividing theindividual corrected component areas by the total correctedarea. Make corrections to account for water and acidity prese
42、ntas determined in accordance with Test Methods D1364 andD1613.NOTE 4Peak areas may be determined by any method that meets theprecision limits given in Section 12. Methods found to be acceptable areplanimetering and integration.10.2 Calculate the weight percent W of each component asfollows:W 5 A/B!
43、 3 100 2 C! (1)where:A = corrected peak response,B = sum of corrected peak responses, andC = sum of water and acidity.11. Report11.1 Report the following information: weight percent ofmethyl isobutyl ketone and any impurities of interest to thenearest 0.01 % absolute. Duplicate runs for major compon
44、entsthat agree within 0.05 % absolute are acceptable for averaging(95 % confidence level).12. Precision and Bias612.1 PrecisionThe precision statements are based upon aninterlaboratory study in which one operator in six differentlaboratories analyzed two samples of methyl isobutyl ketone induplicate
45、 on two days. One sample represented commercialmaterial having a purity of 99.8 % and containing 0.03 %methyl isobutyl carbinol and the other was prepared by adding0.28 % of methyl isobutyl carbinol to the first sample. Theresults were analyzed in accordance with Practice E180.Because one laboratory
46、 failed to report trace impurities, theirresults were omitted from the calculation of the precisionstatements. The within-laboratory standard deviation andbetween-laboratory standard deviation were found to be asfollows:WithinLaboratoryBetweenLaboratoryMethyl isobutyl ketone 0.014 0.078Methyl isobut
47、yl carbinol 0.011 0.044Degrees of freedom 10 4Based upon these standard deviations, the following criteriashould be used for judging the acceptability of results at the95 % confidence level for methyl isobutyl ketone having apurity of 99 to 100 % and containing from 0.0 to 0.5 % of theimpurity methy
48、l isobutyl carbinol.12.1.1 RepeatabilityTwo results, each the mean ofduplicates, obtained by the same operator on different daysshould be considered suspect if they differ by more than 0.05 %absolute for methyl isobutyl ketone or 0.03 % absolute formethyl isobutyl carbinol.12.1.2 ReproducibilityTwo
49、results, each the mean ofduplicates, obtained by operators in different laboratoriesshould be considered suspect if they differ by more than 0.30 %4Messner, A. E., et al, Analytical Chemistry, Vol 31, 1959, pp. 230233.5Dietz, W.A., Journal of Gas Chromatography, Vol 5, No. 2, February 1967, pp.6871.6Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D01-1042. ContactASTM CustomerService at serviceastm.org.D3329 03 (2017)3absolute for methyl isobutyl ketone or 0.17 % absolute
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