1、Designation: D7090 04 (Reapproved 2010)Standard Test Method forPurity of Isophorone by Capillary Gas Chromatography1This standard is issued under the fixed designation D7090; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year
2、 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 purityof isophorone. This method also determines the impurities o
3、fthe material in concentration level less than 0.5 mass %, whichmay include mesityl oxide (MSO), mesityl oxide-isomer,mesitylene, trimethyl cyclohexenone (TMCH), phorone,phorone-isomer, xylitone, and tetralone.1.2 Water cannot be determined by this test method andshall be measured by other appropria
4、te ASTM procedure. Theresult is used to normalize the chromatographic data deter-mined by this test method.1.3 For purposes of determining conformance of an ob-served or a calculated value using this test method to relevantspecifications, test result(s) shall be rounded off “to the nearestunit” in t
5、he last right-hand digit used in expressing thespecification limit, in accordance with the rounding - offmethod of Practice E29.1.4 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
6、appro-priate safety and health practices and to determine theapplicability of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1364 Test Method for Water in Volatile Solvents (KarlFischer Reagent Titration Method)E29 Practice for Using Significant Digits in Test Data t
7、oDetermine Conformance with SpecificationsE300 Practice for Sampling Industrial Chemicals3. Summary of Test Method3.1 A representative specimen is introduced into a gaschromatograph with a bonded polyethylene glycol capillarycolumn using temperature programming and a flame ionizationdetector. The co
8、ncentrations of the sample components arecalculated from the integrated component peaks using internalstandardization technique with response factors. Water ismeasured in accordance with Test Method D1364 and theresult is used to normalize the values obtained by gas chroma-tography.4. Significance a
9、nd Use4.1 This test method determines the purity of isophorone, aswell as the concentration of various potential impurities,several of which are critical in the application of these solvents.5. Apparatus5.1 ChromatographAny gas chromatograph utilizing acapillary column and has the following characte
10、ristics (seeTable 1 for typical GC parameters):5.1.1 DetectorA flame ionization detector (FID) capableof continuous operation at a temperature equivalent to themaximum column temperature employed. The detector shallhave sufficient sensitivity to detect 0.001 mass % of impurity inthe specimen at a pe
11、ak height 3 times the noise level.5.1.2 Columnfused silica capillary column with bondedpolyethylene (see Table 1 for details).5.1.3 Column Temperature ProgrammingThe chromato-graph shall be capable of reproducible linear temperatureprogramming.5.1.4 Sample Inlet SystemThe sample inlet system shallbe
12、 capable of split injection, typically at a 100:1 split ratio.NOTE 1An autoinjector is recommended. Manual injection with asyringe is acceptable, however the observed precision may not apply.5.1.5 IntegratorMeans shall be provided for determiningthe area of the observed chromatographic peaks. This c
13、an bedone by means of an electronic integrator or a computer basedchromatography data system. The integrator/computer systemshall have standard chromatographic software for determiningthe retention times and quantification of eluting peaks.1This test method is under the jurisdiction of ASTM Committe
14、e 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 Dec. 1, 2010. Published December 2010. Originallyapproved in 2004. Last previous edition approved in 2
15、004 as D7090 - 04. DOI:10.1520/D7090-04R10.2For 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 the standards Document Summary page onthe ASTM website.1Copyright ASTM In
16、ternational, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.1.6 Flow ControllerThe chromatograph shall beequipped with a constant flow device capable of maintainingthe carrier gas at a constant flow rate throughout the tempera-ture program.5.1.7 MicrosyringeA m
17、icrosyringe of appropriate capac-ity is required for injection of the specimen into the chromato-graph. Typically,a5Lsyringe is used.6. Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall beused in the preparation of the calibration mixture.6.2 Calibration Mixture Components:6.
18、2.1 Isophoronesolvent used in the preparation of thecalibration mixture, and shall be free of the components ofinterest. If pure isophorone is not available, then isophoronecontaining relatively low concentration of the components ofinterest can be used, and the composition of the calibrationmixture
19、 corrected for components already present.(WarningIsophorone is a cancer suspect agent.)6.2.2 Mesitylene Oxide (MSO), 4-methyl-3-pentene-2-onecalibration component.NOTE 2This chemical is commercially available typically as a mix-ture of two isomers with an MSO to MSO-isomer ratio of 10:1.6.2.3 Mesit
20、ylene Oxide Isomer (MSO-isomer), 4-methyl-4-pentene-2-onecalibration component.6.2.4 Mesitylene, 1,3,5-trimethyl benzenecalibration com-ponent.6.2.5 Trimethyl cyclohexenone (TMCH), 3,5,5-trimethyl-3-cyclohexen-1-one calibration component.6.2.6 Phorone, 2,6-dimethyl-hepta-3,5-diene-2-one cali-bration
21、 component.6.2.7 Phorone - Isomer, 4-6-dimethyl-hepta-3,5-diene-2-one calibration component.NOTE 3This chemical is not commercially available but comes as animpurity of phorone.6.2.8 Tetralone, 3,4-dihydro-1-napthalenonecalibrationcomponent.6.2.9 Xylitone(s)optional calibration component.6.2.10 Deca
22、neinternal standard.6.3 Carrier GasesHelium or hydrogen (minimum99.95 % purity). (WarningHelium and hydrogen are com-pressed gases under high pressure. Hydrogen is highly flam-mable.)7. Sampling7.1 Take samples of the material to be tested using proce-dures described in Practice E300.8. Conditioning
23、 of Capillary Column8.1 Condition the gas chromatographic capillary columnfollowing the column supplier recommendation.9. Calibration and Standardization9.1 Prepare a calibration mixture containing approximately0.1 mass % of each of the components of interest and thedecane internal standard in pure
24、isophorone. The total weightof the calibration mixture solution should be 100 g. If pureisophorone is not available, then isophorone containing rela-tively low concentration of the components of interest can beused, and the composition of the calibration mixture correctedfor components already prese
25、nt. Typical components suitablefor the calibration mixture are: MSO, MSO-isomer, mesity-lene, TMCH, phorone, phorone isomer, xylitone, and tetralone(see 6.2).9.2 Record the actual weight of each added component, theinternal standard, and the total weight of the calibrationmixture.9.3 Determine the d
26、etector response factor of the variouscomponents of interest, by injecting 1 L of the calibrationmixture into a GC using the typical chromatographic param-eters given in Table 1, and using the equation:Fi5Wi3 Ais!Wis3 Ai!(1)where:Fi= detector response factor for the component of inter-est,Wi= weight
27、 of the component of interest in the calibrationmixture, in grams,Wis= weight of the internal standard in the calibrationmixture, in grams,Ai= peak area of the component of interest in thecalibration mixture, andAis= peak area of the internal standard in the calibrationmixture.NOTE 4Most chromatogra
28、phic data systems are capable of determin-ing the detector response factors automatically by inputting the weight orconcentration of the components of interest and the internal standard.10. Procedure10.1 Sample PreparationTare an 8-oz bottle or suitablecontainer with a cap. Using a syringe or an app
29、ropriatedispensing device, add approximately 0.1g (130 L) of theinternal standard (decane). Record the exact weight (Wisx)ofthe added internal standard. Add the material to be tested togive a total weight of the prepared sample of 100.0 6 0.1 g.Record the exact weight of the prepared sample (Wisx).
30、Cap thecontainer, and mix the solution thoroughly.10.2 Sample AnalysisInject 1 L of the prepared sampleinto a GC operating with the typical parameters given in Table1. Obtain the chromatogram of the sample and determine theareas of all the eluted peaks except the isophorone peak usingan appropriate
31、integration device or a chromatographic dataTABLE 1 Typical GC ParametersParameters ValuesColumn 30 m 3 0.32 mm fused silica capillary columnwith 0.5 micron bonded phase polyethyleneglycolColumn Temperature 50C for 5 min., programmed to 210C at 10C/min. Hold for 10 min.Injector Temperature 230CSampl
32、e size 1 LSplit ratio 100:1Detector Flame IonizationDetector Temperature 250CCarrier Gas (Helium) 30 cm/sHydrogen Gas 30 mL/min.Air 300 mL/min.D7090 04 (2010)2system. Table 2 gives typical retention times of the variousimpurity components.Atypical chromatogram is shown in Fig.1. Determine the concen
33、tration of each component detectedusing the chromatographic data system or the followingequation:Cx, in mass % 5Ax3 Fi3 Wisx!Aisx3 Ws!3 100 (2)where:Cx= concentration of the component of interest, mass %,Ax= peak area of the component of interest in thesample,Aisx= peak area of the internal standard
34、 in the sample,Wisx= weight of the internal standard in the sample, ingrams,Ws= weight of the prepared sample for analysis, ingrams, andFi= detector response factor for the component ofinterest as determined in 9.3.10.3 To determine the concentration of unknown peaks, usea response factor of 1.0.11.
35、 Calculation11.1 Calculate the total concentration of the impurities ofisophorone as follows:Ct, mass % 5 ( Cx(3)where:(Cx= sum total of all the concentration of the impuritycomponents.TABLE 2 Typical Retention Times of ChromatographicComponentsComponent Approximate Retention Times (min.)Decane (Int
36、ernal Standard) 8.03MSO-isomer 9.96MSO 11.67Mesitylene 13.88TMCH 16.57Phorone 18.46Phorone-isomer 18.62Isophorone 19.83Xylitone 20.86Tetralone 28.35FIG. 1 Typical Isophorone ChromatogramD7090 04 (2010)311.2 Calculate the purity of isophorone as follows:Purity of isophorone, mass % 5 100 2 Ct1 mass %
37、 water! (4)where:Ct= total concentration of the impurities asdetermined in 11.1, andmass % water = concentration of water determined by TestMethod D1364.12. Report12.1 Report the individual impurity components, if re-quired, to the nearest 0.001 mass %.12.2 Report the isophorone purity to the neares
38、t 0.1 mass %.13. Precision and Bias13.1 PrecisionA preliminary precision statement underrepeatability conditions has been determined by one laboratory,using one calibration mixture sample and 16 replicate deter-minations by one technician on the same day.13.1.1 Table 3 gives the standard deviations
39、for the variousimpurities and isophorone.13.1.2 Reproducibility statement is not available at thepresent time. It will be determined within 5 years after themethod has been approved.13.2 BiasBias cannot be determined for this methodbecause there is no available material with an acceptedreference val
40、ue.14. Keywords14.1 capillary GC; gas chromatography; hydrocarbon sol-vents.; isophoroneASTM International takes no position 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
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43、nts have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown 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 m
44、ultiple 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.a
45、stm.org/COPYRIGHT/).TABLE 3 Repeatability Standard DeviationsComponent Level (mass %) Standard Deviation(mass %)MSO-isomer 0.006 0.0001MSO 0.065 0.0013Mesitylene 0.058 0.0004TMCH 0.080 0.0116Phorone 0.058 0.0018Phorone-isomer - -Xylitone - -Tetralone 0.067 0.0010Isophorone Purity 99.8 0.03D7090 04 (2010)4
