1、Designation: E 202 05Standard Test Methods forAnalysis of Ethylene Glycols and Propylene Glycols1This standard is issued under the fixed designation E 202; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision.
2、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. Scope1.1 These test methods cover the chemical and physicala
3、nalysis of the commonly available grades of ethylene glycol,diethylene glycol, triethylene glycol, propylene glycol, anddipropylene glycol. The key sections appear in the followingorder:SectionsPurity of Reagents 4Specific Gravity 6-8Distillation Range 9-11Acidity 12-14Water 15-17Iron 18-26Color 27-
4、29Gas Chromatographic Analysis 30-401.2 Review the current appropriate Material Safety DataSheets (MSDS) for detailed information concerning toxicity,first aid procedures, and safety precautions.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use.
5、 It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 891 Test Methods for Specific Gravity, Apparent, ofLiquid Industrial Chemic
6、alsD 1078 Test Method for Distillation Range of VolatileOrganic LiquidsD 1193 Specification for Reagent WaterD 1209 Test Method for Color of Clear Liquids (Platinum-Cobalt Scale)D 1613 Test Method for Acidity in Volatile Solvents andChemical Intermediates Used in Paint, Varnish, Lacquer,and Related
7、ProductsD 4052 Test Method for Density and Relative Density ofLiquids by Digital Density MeterD 5386 Test Method for Color of Liquids Using TristimulusColorimetryE60 Practice for Photometric and SpectrophotometricMethods for Chemical Analysis of MetalsE 180 Practice for Determining the Precision of
8、ASTMMethods for Analysis and Testing of Industrial ChemicalsE 200 Practice for Preparation, Standardization, and Stor-age of Standard and Reagent Solutions for ChemicalAnalysisE 203 Test Method for Water Using Karl Fischer ReagentE 394 Test Method for Iron in Trace Quantities Using the1,10-Phenanthr
9、oline MethodE611 Test Methods for Low Concentrations of DiethyleneGlycol in Ethylene Glycol by Gas ChromatographyE 1064 Test Method for Water in Organic Liquids byCoulometric Karl Fischer TitrationE 1615 Test Method for Iron in Trace Quantities Using theFerroZine MethodE 2409 Test Method for Glycol
10、Impurities in Mono-, Di-,Tri-, and Tetraethylene Glycol (Gas ChromatographicMethod)3. Significance and Use3.1 These test methods measure certain chemical and physi-cal properties of ethylene glycols and propylene glycols andmay be used to determine compliance with specification inwhich limits are es
11、tablished for these properties. For those teststhat use the procedure of another ASTM test method, that testmethod should be consulted for additional information on thesignificance and use of that test.3.2 Alternative test methods and technology for several ofthe methods can be found in the Appendix
12、. The alternative testmethods do not have precision data for the application of these1These test methods are under the jurisdiction of ASTM Committee E15 onIndustrial and Specialty Chemicals and are the direct responsibility of Subcommit-tee E15.01 on General Standards.Current edition approved Oct.
13、1, 2005. Published November 2005. Originallyapproved in 1962. Last previous edition approved in 2004 as E 20204.2For 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
14、standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.methods in analyzing glycols. Use of these methods is optionaland individuals using the alternative methods should assurethemselves th
15、at the method is sufficiently precise. Precisiondata presented is only for the original test methods listed.4. Purity of Reagents4.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of
16、 the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.3Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.4.2 Unless ot
17、herwise indicated, references to water shall beunderstood to mean reagent water conforming to SpecificationD 1193, Type II or III.5. Quality Control5.1 It is recommended that a control chart for the concen-tration of the impurities in the glycol quality control sample beestablished and maintained ac
18、cording to common guidelines.4Measure the control sample each time a test sample(s) is tested.If the measured value exceeds the action limit of the controlchart, take appropriate action before proceeding with sampletests.SPECIFIC GRAVITY6. Procedure6.1 Determine the relative density of the sample at
19、 20/20Cusing the pycnometer test method in accordance with TestMethods D 891, except determine the water and sampleweights of the pycnometer at 20.0 6 0.1C.7. Report7.1 Report the relative density at 20/20C (in air) to thenearest 0.0001 unit.8. Precision and Bias8.1 The following criteria should be
20、used for judging theacceptability of results (see Note 1):8.1.1 Repeatability (Single Analyst)The standard devia-tion for a single determination has been estimated to be0.0000651 unit at 96 dF. The 95 % limit for the differencebetween two such runs is 0.0002 unit.8.1.2 Laboratory Precision (Within-L
21、aboratory, Between-Days)The standard deviation of results (each the average ofduplicates), obtained by the same analyst on different days, hasbeen estimated to be 0.0000598 units at 48 df. The 95 % limitfor the difference between two such averages is 0.0002 unit.8.1.3 Reproducibility (Multilaborator
22、y)The standard de-viation of results (each the average of duplicates), obtained byanalysts in different laboratories, has been estimated to be0.000191 unit at 5 dF. The 95 % limit for the differencebetween two such averages is 0.0005 unit.NOTE 1These precision estimates are based on interlaboratory
23、studiesperformed in 1962 and 1963 on six samples of the five glycols whosespecific gravity values range from approximately 1.0233 to 1.1255.Atotalof ten laboratories cooperated in the studies in which each analystperformed duplicate determinations on each sample on each of two days.5Practice E 180 w
24、as used in developing these precision estimates.8.2 BiasThe bias of this test method has not been deter-mined due to the unavailability of suitable reference materials.DISTILLATION RANGE9. Procedure9.1 Determine the distillation range of the sample in accor-dance with Test Method D 1078. Use the con
25、ditions as speci-fied in Test Method D 1078, and the ASTM Solvents Distilla-tion Thermometer shown in Table 1. (See Note 2 for certainallowable exceptions in applying this test method to triethyleneglycol.)NOTE 2In the distillation of triethylene glycol, it may not be possibleto collect the first dr
26、op of liquid within 15 min or to maintain theprescribed distillation rate of 4 to 5 mL/min with some sources of gas. Inthis case, up to 30 min can be allowed to collect the first drop, and adistillation rate of 2 to 3 mL/min is satisfactory. Alternatively, the flaskchamber may be covered with a suit
27、able shield so that only the upper neckand thermometer are exposed to room air to achieve the specified rates.9.2 Use the following values of K in the equation forbarometric correction (Test Method D 1078):Chemical KEthylene glycol 0.045Diethylene glycol 0.050Triethylene glycol 0.055Propylene glycol
28、 0.043Dipropylene glycol 0.05110. Report10.1 Report the corrected temperatures to the nearest 0.1Cat each volume required by the specification for the glycolbeing analyzed.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the t
29、esting of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, VWR International Ltd., Poole, Dorset, U.K., and the United StatesPharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc.(USPC), Rockville, MD.4ASTM Manual on Presentation of
30、 Data and Control Chart Analysis, 7thEdition, ASTM Manual Series MNL 7A (revision of Special Technical Publication(STP) 15D).5Details of the interlaboratory study are available as Research Report E15-0013from ASTM Headquarters.TABLE 1 Thermometers for Distillation RangeGlycolThermometerNumberThermom
31、eterRangeEthylene glycol 104C 173 to 227CDiethylene glycol 106C 223 to 277CTriethylene glycol 107C 248 to 302CPropylene glycol 104C 173 to 227CDipropylene glycol 106C 223 to 277CE20205211. Precision and Bias11.1 The following criteria should be used for judging theacceptability of results (Note 3):1
32、1.1.1 Repeatability (Single Analyst)The standard devia-tion for a single determination has been estimated to be thevalue in Table 2 at the indicated degrees of freedom. The 95 %limit for the difference between two such runs is the value inthe table.11.1.2 Laboratory Precision (Within-Laboratory, Bet
33、ween-Days)The standard deviation of results (each the average ofduplicates), obtained by the same analyst on different days, hasbeen estimated to be the value in Table 2 at the indicateddegrees of freedom. The 95 % limit for the difference betweentwo such averages is the value in the table.11.1.3 Re
34、producibility (Multilaboratory)The standard de-viation of results (each the average of duplicates), obtained byanalysts in different laboratories, has been estimated to be thevalue in Table 2 at the indicated degrees of freedom. The 95 %limit for the difference between two such averages is the value
35、in the table.NOTE 3These precision estimates are based on interlaboratory studiesperformed in 1962 and 1963 on eleven samples of the five glycols whosedistillation ranges varied from 1.4 to 9.7C. A total of ten laboratoriescooperated in the studies in which each analyst performed duplicatedeterminat
36、ions on each sample on each of two days.5Practice E 180 wasused in developing these precision estimates.11.2 BiasThe bias of this test method has not beendetermined due to the unavailability of suitable referencematerials.ACIDITY12. Procedure12.1 Determine the acidity of the sample in accordance wit
37、hTest Method D 1613.13. Report13.1 Report the acidity, expressed as mass percent of aceticacid, to the nearest 0.0001 %.14. Precision and Bias14.1 The following criteria should be used for judging theacceptability of results (see Note 4):14.1.1 Repeatability (Single Analyst)The standard devia-tion f
38、or a single determination has been estimated to be0.0000918 % absolute at 92 dF. The 95 % limit for thedifference between two such runs is 0.0003 % absolute.14.1.2 Laboratory Precision (Within-Laboratory, Between-Days)The standard deviation of results (each the average ofduplicates), obtained by the
39、 same analyst on different days, hasbeen estimated to be 0.000116 % absolute at 46 dF. The 95 %limit for the difference between two such averages is 0.0003 %absolute.14.1.3 Reproducibility (Multilaboratory)The standard de-viation of results (each the average of duplicates), obtained byanalysts in di
40、fferent laboratories, has been estimated to be0.000279 % absolute at 5 df. The 95 % limit for the differencebetween two such averages is 0.0008 % absolute.NOTE 4These precision estimates are based on an interlaboratorystudy performed in 1962 and 1963 on six samples of the five glycolswhose acidity v
41、alues ranged from 0.0008 to 0.0044 %. A total of tenlaboratories cooperated in the studies in which each analyst performedduplicate determinations on each of two days.5Practice E 180 was used indeveloping these precision estimates.TABLE 2 Distillation Range Precision ValuesEthylene GlycolDistillatio
42、n RangeDiethyleneandTriethyleneGlycolsPropyleneandDipropyleneGlycols0 to 5C/qa 5 to 15CInitial boiling point, C:RepeatabilityStandard deviation 0.154 (54A) 0.154 (54) 0.218 (52) 0.148 (56)95 % limit 0.4 0.4 0.6 0.4Laboratory Precision(Within LaboratoryBetween Days)Standard deviation 0.173 (27) 0.173
43、 (27) 0.119 (23) 0.0901(28)95 % limit 0.5 0.5 0.4 0.2ReproducibilityStandard deviation 0.414 (8) 0.414 (8) 0.489 (6) 0.190 (6)95 % limit 1.2 1.2 1.4 0.55 mL, C:RepeatabilityStandard deviation 0.118 (54) 0.118 (54) . .95 % limit 0.3 0.3 . .Laboratory Precision(Within LaboratoryBetween Days)Standard d
44、eviation 0.147 (27) 0.147 (27) . .95 % limit 0.4 0.4 . .ReproducibilityStandard deviation 0.317 (8) 0.317 (8) . .95 % limit 0.9 0.9 . .50 mL, C:RepeatabilityStandard deviation 0.0783 (54) 0.0783(54) 0.129 (52) 0.0892(56)95 % limit 0.2 0.2 0.4 0.2Laboratory Precision(Within LaboratoryBetween Days)Sta
45、ndard deviation 0.0981 (27) 0.0981(27) 0.0961(26) 0.0505(28)95 % limit 0.3 0.3 0.3 0.1ReproducibilityStandard deviation 0.279 (8) 0.279 (8) 0.201 (6) 0.133 (6)95 % limit 0.8 0.8 0.6 0.495 mL, C:RepeatabilityStandard deviation 0.0837 (54) 0.0837(54) . .95 % limit 0.2 0.2 . .Laboratory Precision(Withi
46、n LaboratoryBetween Days)Standard deviation 0.126 (27) 0.126 (27) . .95 % limit 0.4 0.4 . .ReproducibilityStandard deviation 0.336 (8) 0.336 (8) . .95 % limit 0.9 0.9 . .Dry point C:RepeatabilityStandard deviation 0.0779 (14) 0.384 (36) 0.272 (46) 0.193 (56)95 % limit 0.2 1.1 0.8 0.5Laboratory Preci
47、sion(Within LaboratoryBetween Days)Standard deviation 0.122 (8) 0.640 (18) 0.103 (23) 0.250 (28)95 % limit 0.3 1.8 0.3 0.7ReproducibilityStandard deviation 0.466 (7) 2.77 (8) 1.12 (5) 0.896 (6)95 % limit 1.3 7.8 3.1 2.5ADegrees of freedom indicated by values within parentheses.E20205314.2 BiasThe bi
48、as of this test method has not beendetermined due to the unavailability of suitable referencematerials.WATER15. Procedure15.1 Determine the water content of the sample using anysuitable Karl Fischer reagent titration method. Test MethodE 203 is recommended.16. Report16.1 Report the water content to
49、the nearest 0.01 % mass.17. Precision and Bias17.1 The following criteria should be used for judging theacceptability of results (see Note 5):17.1.1 Repeatability (Single Analyst)The standard de-viation for a single determination has been estimated to be0.000370 % absolute at 92 dF. The 95 % limit for the differencebetween two such runs is 0.01 % absolute.17.1.2 Laboratory Precision (Within-Laboratory, Between-Days)The standard deviation of results (each the average ofduplicates), obtained by the same analyst on different days, hasbeen estimated to b
