ASTM D2804-2002(2007) Standard Test Method for Purity of Methyl Ethyl Ketone By Gas Chromatography《气相色谱法测定丁酮纯度的标准试验方法》.pdf

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1、Designation: D 2804 02 (Reapproved 2007)Standard Test Method forPurity of Methyl Ethyl Ketone By Gas Chromatography1This standard is issued under the fixed designation D 2804; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the yea

2、r 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.This standard has been approved for use by agencies of the Department of Defense.1. Scope*1.1 This test method covers the de

3、termination of the purityof methyl ethyl ketone by gas chromatography. Impuritiesincluding water, acidity, and nonvolatile matter are measuredby appropriate ASTM procedures and the results are used tonormalize the chromatographic value.1.2 For purposes of determining conformance of an ob-served valu

4、e or a calculated value using this test method torelevant specifications, test result(s) shall be rounded off “tothe nearest unit” in the last right-hand digit used in expressingthe specification limit, in accordance with the rounding-offmethod of Practice E29.1.3 The values stated in SI units are t

5、o be regarded asstandard. No other units of measurement are included in thisstandard.1.4 For hazard information and guidance, see the suppliersMaterial Safety Data Sheet.2. Referenced Documents2.1 ASTM Standards:2D 1353 Test Method for Nonvolatile Matter in VolatileSolvents for Use in Paint, Varnish

6、, Lacquer, and RelatedProductsD 1364 Test Method for Water in Volatile Solvents (KarlFischer Reagent Titration Method)D 1613 Test Method for Acidity in Volatile Solvents andChemical Intermediates Used in Paint, Varnish, Lacquer,and Related ProductsD 2593 Test Method for Butadiene Purity and Hydrocar

7、bonImpurities by Gas ChromatographyD 4626 Practice for Calculation of Gas ChromatographicResponse FactorsE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE 180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industria

8、l and Spe-cialty Chemicals3. Summary of Test Method3.1 A representative specimen is introduced into a gas-chromatographic column. The methyl ethyl ketone is separatedfrom other impurities such as hydrocarbons, alcohols, acetone,di-sec-butyl ether, and ethyl acetate as the components aretransported t

9、hrough the column by an inert carrier gas. Theseparated components are measured in the effluent by adetector and recorded as a chromatogram. The chromatogramis interpreted by applying component-attenuation and detector-response factors to the peak areas, and the relative concentra-tion is determined

10、 by relating individual peak response to thetotal peak response. Water, acidity, and nonvolatiles are mea-sured by the procedures listed in 3.2, and the results are usedto normalize the results obtained by gas chromatography.3.2 The appropriate ASTM test methods are:3.2.1 WaterTest Method D 1364.3.2

11、.2 AcidityTest Method D 1613.3.2.3 Nonvolatile MatterTest Method D 1353.4. Significance and Use4.1 This test method provides a measurement of commonlyfound impurities in commercially available methyl ethyl ke-tone. The measurement of these impurities and the resultsthereof can individually or when t

12、otaled and subtracted from100 (assay) be used for specification purposes.5. Apparatus5.1 ChromatographAny gas chromatograph having eithera thermal-conductivity or flame ionization detector providedthe system has sufficient sensitivity and stability to obtain for0.01 weight % of impurity a recorder d

13、eflection of at least 2mm at a signal-to-noise ratio of at least 5 to 1. The specimensize to be used in judging the sensitivity must be such that thecolumn is not overloaded.5.2 ColumnAny column capable of resolving methylethyl ketone from the impurities that may be present. Possibleimpurities are p

14、araffins, acetone, methanol, ethanol, propanol,isopropanol, tert-butanol, sec-butanol, di-sec-butyl ether, and1This 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

15、, Plasticizers, and Chemical Intermediates.Current edition approved June 1, 2007. Published June 2007. Originallyapproved in 1969. Last previous edition approved in 2002 as D 2804 02.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.

16、org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.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 Stat

17、es.ethyl acetate. The peaks should be resolved, quantitatively inproportion to concentration, within a practical elapsed time.Columns that meet the requirements of this test method arelisted in Table 1. Other columns may be used, provided the userestablishes that a column gives the required separati

18、on and theprecision requirements of Section 13 are met.5.3 Specimen Introduction SystemAny specimen systemcapable of introducing a representative specimen into thecolumn may be used. Systems that have been used successfullyto introduce 1 to 10-L of methyl ethyl ketone specimensinclude microlitre syr

19、inges, micropipets, and liquid samplingvalves.5.4 RecorderAn electronic integrator or a recording po-tentiometer with a full-scale deflection of 5 mV or less,full-scale response time of 2 s or less, and sufficient sensitivityto meet the requirements of 5.1.6. Reagents and Materials6.1 Carrier Gas, a

20、ppropriate to the type of detector used.Helium or hydrogen may be employed with thermal conduc-tivity detectors, and nitrogen, helium, or argon with ionizationdetectors. The minimum purity of any carrier should be 99.95mol %.6.1.1 WarningIf hydrogen is used, take special safetyprecaution to ensure t

21、hat the system is free of leaks and that theeffluent is vented properly.6.2 Column Materials:6.2.1 Liquid PhaseThe materials successfully used incooperative work as liquid phases are listed in Table 1 (seeNote 1).6.2.2 Solid SupportThe support for use in the packedcolumn is usually (PTFE)-fluorocarb

22、on, crushed firebrick, ordiatomaceous earth. Table 1 lists conditions used successfullyin cooperative work (see Note 1).NOTE 1See research report for additional information, available fromASTM International Headquarters. Request RR:D011107.6.2.3 Tubing MaterialCopper, stainless steel, nickel cop-per

23、 alloy, aluminum, and various plastic materials have beenfound to be satisfactory for column tubing. The material mustbe nonreactive with the substrate, sample, and carrier gas.6.3 Standards for Calibration and IdentificationStandardsamples for all components present are needed for identifica-tion b

24、y retention time, and for calibration for quantitativemeasurements (Note 2).NOTE 2Mixtures of components may be used, provided there is nouncertainty as to the identity or concentration of compounds involved.7. Preparation of Apparatus7.1 Column PreparationThe method used to prepare thecolumn is not

25、 critical provided that the finished columnproduces the required separation (Note 3). Partitioning liquids,supports, and loading levels used successfully in cooperativework are listed in Table 1. These may be obtained from mostchromatography supply houses.NOTE 3A suitable method for column preparati

26、on is described in TestMethod D 2593.7.2 ChromatographInstall the column in the chromato-graph and establish the operating conditions required to givethe desired separation. Relative component retention times,along with the typical retention time for methyl ethyl ketoneare listed in Table 1. Allow s

27、ufficient time for the instrument toreach equilibrium as indicated by a stable recorder baseline.TABLE 1 Columns and Conditions Used Successfully in Cooperative WorkCase I Case II Case III Case IV Case V Case VIColumn:Liquid phasepackedpolyethyleneglycol 1500packedpolyethyleneglycol 400packedpolyeth

28、yleneglycol 300packedpolyethyleneglycol 200packedpolyethyleneglycol 1500capillarypolytrifluoro-propylsiloxaneLiquid phase, weight % 10 28 20 20 20 1.2 m filmSupport type TFE resin Pink, diato-maceous earthPink, diato-maceous earthWhite, diato-maceous earthPink, diato-maceous earthnoneSupport mesh si

29、ze 40/60 30/60 40/60 60/80 60/80 .Length, ft (m) 12 (3.7) 18 (5.5) 10 (3.0) 10 (3.0) 20 (6.1) 32.8 (10.0)Outside diameter, in. (mm) 0.25 (6.4) 0.25 (6.4) 0.25 (6.4) 0.125 (3.2) 0.25 (6.4) 0.028 (0.72)Inside diameter, in. (mm) 0.21 (5.3) 0.21 (5.3) 0.21 (5.3) 0.085 (2.2) 0.21 (5.3) 0.021 (0.53)Column

30、 temperature, C 100 80 75 70 100 30Carrier gas helium helium helium helium helium heliumCarrier flow rate, mL/min 60 80 35 60 50 3.7Typical retention time, minmethyl ethyl ketone6.9 17.0 11.0 5.8 16.5 8.8Relative retention time(methyl ethyl ketone = 1.00):Propyl ether 0.19 0.14 . . . .Octenes 0.54 0

31、.21 . 0.34 . 0.65sec-Butyl ether 0.78 0.45 . 0.47 1.21 .Acetone 0.61 0.54 0.64 0.67 0.67 0.60Ethyl acetate 0.81 . 0.82 0.78 0.85 0.78Methyl ethyl ketone 1.00 1.00 1.00 1.00 1.00 1.00tert-Butanol 1.00 1.12 1.27 1.71 1.03 0.39Methanol 1.10 . 1.36 1.71 1.09 0.27Isopropanol 1.20 1.32 . 2.03 2.12 0.34Eth

32、anol 1.30 . 1.73 2.21 1.27 0.31sec-Butanol 2.12 2.26 2.73 3.50 1.94 0.53n-Propanol 2.35 . 3.27 3.97 . 0.43D 2804 02 (2007)28. Calibration and Standardization8.1 IdentificationSelect the conditions of column tem-perature and carrier-gas flow that will give the necessarycomponent resolution. Determine

33、 the retention time for eachcomponent by injecting small amounts of the compound eitherseparately or in mixtures.8.2 StandardizationThe area under the peak of the chro-matogram is considered a quantitative measure of the amountof the corresponding compound. The relative area is propor-tional to the

34、concentrations if the detector responds equally toall of the sample components. Differences in detector responsemay be corrected by use of relative response factors obtainedby injecting and measuring the response to pure (99 weight %minimum) compounds or known blends. It is permissible touse the est

35、ablished response factors shown in Table 2 instead ofstandardization.8.3 In using literature values, area response from thermal-conductivity detectors is corrected by multiplying each com-ponent area by the respective weight factor above.NOTE 4It must be recognized that the use of published response

36、factors serves only as a rough estimate, due to differences in equipmentgeometry, condition, and types of detectors. It is preferable for eachanalyst to determine actual response factors on his own instrument. Referto Practice D 4626 for calculation of gas chromatographic response factor.NOTE 5When

37、thermal-conductivity detectors are used for the analysisof high-purity methyl ethyl ketone, the difference between area percent iswithin the precision of the method.9. Procedure9.1 Using a suitable method selected from 5.3, introducesufficient representative liquid specimen into the chromato-graph t

38、o ensure a minimum of 10 % recorder deflection for a0.1 % concentration of impurity at the most sensitive-operatingsetting of the instrument.9.2 Using the same conditions as for component identifica-tion and standardization, record the peaks of all compounds atattenuation settings that provide maxim

39、um peak heights.10. Calculation10.1 Measure the area of all peaks (Note 6) and multiply bythe appropriate attenuation factor to express the peak areas ona common basis. If a flame ionization detector was used, applythe appropriate detector-response factors to correct for thedifference in response to

40、 the components. Calculate the weightpercent composition by dividing the individual correctedcomponent areas by the total corrected area. Make correctionsto account for the water, acidity, and nonvolatile matter asdetermined by the ASTM procedures given in 3.1.NOTE 6Peak areas may be determined by a

41、ny method that meets theprecision limits given in Section 12. Methods found to be acceptableinclude planimetering, integration, and triangulation (multiplying the peakheight by the width at the half-height).10.2 Calculate weight percent as follows:Methyl ethyl ketone, weight % 5 A/B! 3 100 2 C! (1)w

42、here:A = corrected peak response,B = sum of corrected peak responses, andC = sum of water, acidity, and nonvolatile impurities.11. Report11.1 Report the following information: weight percent ofmethyl ethyl ketone and any impurities of interest to the nearest0.01 %.12. Precision and Bias12.1 Precisio

43、nThe precision statements are based upon aninterlaboratory study in which one operator in six differentlaboratories analyzed in duplicate on two days two specimensof methyl ethyl ketone from different manufacturers. Theresults were analyzed in accordance with Practice E 180, andthe within-laboratory

44、 standard deviation was found to be0.007 % absolute with 12 degrees of freedom and the between-laboratories standard deviation 0.033 % absolute with fivedegrees of freedom. Based on these standard deviations thefollowing criteria should be used for judging the acceptabilityat the 95 % confidence lev

45、el, of results obtained on methylethyl ketone having a purity of 99 to 100 %:12.1.1 RepeatabilityTwo results each the mean of tworuns obtained by a single analyst on different days should beconsidered suspect if they differ by more than 0.02 % absolute.12.1.2 ReproducibilityTwo results each the mean

46、 of tworuns obtained by analysts in different laboratories should beconsidered suspect if they differ by more than 0.12 % absolute.12.2 BiasBias can not been determined for this testmethod because there is no accepted reference material.13. Keywords13.1 GC; methyl ethyl ketone; purity by gaschromato

47、graphyTABLE 2 Thermal Conductivity DetectorA, BThermalMoleResponseWeightFactorMethyl ethyl ketone 98 0.74Di-n-butyl ether 160 0.81Di-isopropyl ether 130 0.79Ethyl acetate 111 0.79sec-Butanol 97 0.76tert-Butanol 96 0.77Acetone 86 0.68Isopropanol 85 0.71Propanol 83 0.72Ethanol 72 0.64Methanol 55 0.58A

48、The data on the thermal conductivity response are based on data presented byMessner, A. E. et al, Analytical Chemistry, Vol 31, 1959, pp. 230233, and Dietz,W. A., Journal of Gas Chromatography, Vol 5, No. 2, February 1967, pp 6871(see Note 4 of this test method).BFor reference, hydrogen flame respon

49、se data on all compounds except theethers are presented in the above paper by W. A. Dietz.D 2804 02 (2007)3SUMMARY OF CHANGESCommittee D01.35 has identified the location of selected changes to this standard since the last issue(D 2804 - 98) that may impact the use of this standard.(1) Added Practice E29to the Scope section. (2) Added Practice E29to the Referenced Documents section.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard