1、Designation: D 7090 04Standard Test Method forPurity of Isophorone by Capillary Gas Chromatography1This standard is issued under the fixed designation D 7090; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisio
2、n. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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 ofthe material i
3、n 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 appropriate ASTM procedu
4、re. 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 the last right-h
5、and digit used in expressing thespecification limit, in accordance with the rounding - offmethod of Practice E 29.1.4 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 appro-priate s
6、afety and health practices and to determine theapplicability of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1364 Test Method for Water in Volatile Solvents (KarlFischer Reagent Titration Method)E 29 Practice for Using Significant Digits in Test Data toDetermine C
7、onformance with SpecificationsE 300 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 concentration
8、s of the sample components arecalculated from the integrated component peaks using internalstandardization technique with response factors. Water ismeasured in accordance with Test Method D 1364 and theresult is used to normalize the values obtained by gas chroma-tography.4. Significance and Use4.1
9、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 characteristics (s
10、eeTable 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 peak height
11、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 shall becapable o
12、f 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 can bedone
13、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.5.1.6 Flow Controllerthe chromatograph shall beequipped with a constan
14、t flow device capable of maintainingthe carrier gas at a constant flow rate throughout the tempera-ture program.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 Solven
15、ts, Plasticizers, and Chemical Intermediates.Current edition approved Nov. 1, 2004. Published November 2004.2For 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 stan
16、dards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.1.7 Microsyringea microsyringe of appropriate capacityis required for injection of the specimen into the chromato-graph. Typically,a5Lsy
17、ringe 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:6.2.1 Isophoronesolvent used in the preparation of thecalibration mixture, and shall be free of the components ofinterest
18、. If pure isophorone is not available, then isophoronecontaining relatively low concentration of the components ofinterest can be used, and the composition of the calibrationmixture corrected for components already present.(WarningIsophorone is a cancer suspect agent.)6.2.2 Mesitylene Oxide (MSO), 4
19、-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 Mesitylene Oxide Isomer (MSO-isomer), 4-methyl-4-pentene-2-onecalibration component.6.2.4 Mesitylene, 1,3,5-trimethyl benzen
20、ecalibration 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 component.6.2.7 Phorone - Isomer, 4-6-dimethyl-hepta-3,5-diene-2-one calibration component.NOTE 3This chemical is not
21、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 Decaneinternal standard.6.3 Carrier GasesHelium or hydrogen (minimum99.95 % purity). (WarningHelium and hydrogen are com-pr
22、essed 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 E 300.8. Conditioning of Capillary Column8.1 Condition the gas chromatographic capillary columnfollowing the column supplier recommendation
23、.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 isophorone. The total weightof the calibration mixture solution should be 100 g. If pureisophorone is not available, t
24、hen isophorone containing rela-tively low concentration of the components of interest can beused, and the composition of the calibration mixture correctedfor components already present. Typical components suitablefor the calibration mixture are: MSO, MSO-isomer, mesity-lene, TMCH, phorone, phorone i
25、somer, 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 detector response factor of the variouscomponents of interest, by injecting 1 L of the calibrationmixture into a GC usi
26、ng 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 of the component of interest in the calibrationmixture, in grams,Wis= weight of the internal standard in the calibrat
27、ionmixture, 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 chromatographic data systems are capable of determin-ing the detector response factors automatically by inputting the weight orco
28、ncentration 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 appropriatedispensing device, add approximately 0.1g (130 L) of theinternal standard (decane). Record the exact weight (W
29、isx)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 (Ws). Cap thecontainer, and mix the solution thoroughly.10.2 Sample AnalysisInject 1 L of the prepared sampleinto a GC operati
30、ng 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 integration device or a chromatographic datasystem. Table 2 gives typical retention times of the variousTABLE 1 Typical
31、GC ParametersParameters ValuesColumn 30 m x 0.32 mm fused silica capillary columnwith 0.5 micron bonded phase polyethyleneglycolColumn Temperature 50 C for 5 min., programmed to 210 C at 10C/min. Hold for 10 min.Injector Temperature 230 CSample size 1 LSplit ratio 100:1Detector Flame IonizationDetec
32、tor Temperature 250 CCarrier Gas (Helium) 30 cm/sHydrogen Gas 30 mL/min.Air 300 mL/min.D7090042impurity components. A typical chromatogram is shown in Fig.1. Determine the concentration of each component detectedusing the chromatographic data system or the followingequation:Cx, in mass % 5Ax3 Fi3 Wi
33、sx!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 in the sample,Wisx= weight of the internal standard in the sample, ingrams,Ws= weight of the prepared sample for analysis
34、, 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. Calculation11.1 Calculate the total concentration of the impurities ofisophorone as follows:Ct, mass % 5 ( Cx(3)TABLE 2 T
35、ypical Retention Times of ChromatographicComponentsComponent Approximate Retention Times (min.)Decane (Internal 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 ChromatogramD7090043
36、where:(Cx= sum total of all the concentration of the impuritycomponents.11.2 Calculate the purity of isophorone as follows:Purity of isophorone, mass % 5 100 2 Ct1 mass % water! (4)where:Ct= total concentration of the impurities asdetermined in 11.1, andmass % water = concentration of water determin
37、ed by TestMethod D 1364.12. Report12.1 Report the individual impurity components, if re-quired, to the nearest 0.001 mass %.12.2 Report the isophorone purity to the nearest 0.1 mass %.13. Precision and Bias13.1 PrecisionA preliminary precision statement underrepeatability conditions has been determi
38、ned 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 for the variousimpurities and isophorone.13.1.2 Reproducibility statement is not available at thepresent time. It will be determi
39、ned 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 value.14. Keywords14.1 capillary GC; gas chromatography; hydrocarbon sol-vents.; isophoroneASTM International takes no position resp
40、ecting 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 s
41、tandard 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 Interna
42、tional 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 bel
43、ow.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
44、(fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).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 0.03D7090044
