1、Designation: E202 12E202 18Standard Test Methods forAnalysis of Ethylene Glycols and Propylene Glycols1This standard is issued under the fixed designation E202; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revis
2、ion. 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. Scope*1.1 These test methods cover the chemical and
3、 physical analysis of the commonly available grades of ethylene glycol,diethylene glycol, triethylene glycol, propylene glycol, and dipropylene glycol. The key sections appear in the following order:SectionsPurity of Reagents 4Specific Gravity 6 8Distillation Range 9 11Distillation Range 10 12Acidit
4、y 12 14Acidity 14 16Water 15 17Water 18 20Iron 18 20Iron 22 24Color 21 23Color 26 28Gas Chromatographic Analysis 24 26Gas Chromatographic Analysis 30 32Alternative Test Methods Appendix X11.2 Review the current appropriate Material Safety Data Sheets (MSDS)(SDS) for detailed information concerning t
5、oxicity, firstaid procedures, and safety precautions.1.3 In determining the conformance of the test results using this method to applicable specifications, results shall be roundedoff in accordance with the rounding-off method of Practice E29.1.4 The values stated in SI units are to be regarded as s
6、tandard. No other units of measurement are included in this standardwith the exception of foot-pound for apparatus descriptions.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish
7、 appropriate safety safety, health, and healthenvironmental practices and determine theapplicability of regulatory limitations prior to use.1.6 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principl
8、es for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D891 Test Methods for Specific Gravity, Apparent, of Liquid Industrial Chemicals (Withdrawn 2018)
9、3D1078 Test Method for Distillation Range of Volatile Organic LiquidsD1193 Specification for Reagent WaterD1209 Test Method for Color of Clear Liquids (Platinum-Cobalt Scale)1 These test methods are under the jurisdiction of ASTM Committee D16 on Aromatic Hydrocarbons Aromatic, Industrial, Specialty
10、 and Related Chemicals and are thedirect responsibility of Subcommittee D16.15 on Industrial and Specialty General Standards.Current edition approved April 1, 2012March 15, 2018. Published May 2012April 2018. Originally approved in 1962. Last previous edition approved in 20102012 asE20210. DOI: 10.1
11、520/E0202-12. 12. DOI: 10.1520/E0202-18.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The last approved v
12、ersion of this historical standard is referenced on www.astm.org.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all
13、 changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 10
14、0 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1D1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lacquer, and RelatedProductsD4052 Test Method for Density, Relative Density, and API Gravity of Liquids by Digital D
15、ensity MeterD5386 Test Method for Color of Liquids Using Tristimulus ColorimetryD6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related MaterialsE29 Practice for Using Significant Digits in Test Data to Determine Conformance with SpecificationsE180 Prac
16、tice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals(Withdrawn 2009)3E203 Test Method for Water Using Volumetric Karl Fischer TitrationE394 Test Method for Iron in Trace Quantities Using the 1,10-Phenanthroline MethodE611 Test Methods for
17、Low Concentrations of Diethlyene Glycol in Ethylene Glycol by Gas ChromatographyE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test MethodE1064 Test Method for Water in Organic Liquids by Coulometric Karl Fischer TitrationE1510 Practice for Installing Fused Sil
18、ica Open Tubular Capillary Columns in Gas ChromatographsE1615 Test Method for Iron in Trace Quantities Using the FerroZine MethodE2409 Test Method for Glycol Impurities in Mono-, Di-, Tri- and Tetraethylene Glycol and in Mono- and DipropyleneGlycol(Gas Chromatographic Method)E2679 Test Method for Ac
19、idity in Mono-, Di-, Tri- and Tetraethylene Glycol byNon-Aqueous Potentiometric Titration2.2 ASTM Adjuncts:Adjunct ADJD6300 Determination of Precision and Bias for Use in Test Methods for Petroleum Products and Lubricants42.3 Other Document:OSHA Regulations, 29 CFR paragraphs 1910.1000 and 1910.1200
20、53. Significance and Use3.1 These test methods measure certain chemical and physical properties of ethylene glycols and propylene glycols and maybe used to determine compliance with specification in which limits are established for these properties. For those tests that use theprocedure of another A
21、STM test method, that test method should be consulted for additional information on the significance anduse of that test.3.2 Alternative test methods and technology for several of the methods can be found in the Appendix. Use of these methodsis optional and individuals using the alternative methods
22、should assure themselves that the method is sufficient and appropriate forthe application. Precision data presented in this standard is only for the original test methods listed.4. Purity of Reagents4.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated,
23、 it is intended that allreagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, wheresuch specifications are available.6 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently highpurity to permit
24、its use without lessening the accuracy of the determination.4.2 Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to SpecificationD1193, Type II or III.5. Quality Control5.1 It is recommended that a control chart for the concentration of the impurit
25、ies in the glycol quality control sample beestablished and maintained according to common guidelines.7 Measure the control sample each time a test sample(s) is tested. Ifthe measured value exceeds the action limit of the control chart, take appropriate action before proceeding with sample tests.SPEC
26、IFIC GRAVITY6. Procedure6.1 Determine the relative density of the sample at 20/20C using the pycnometer test method in accordance with Test MethodsD891, except determine the water and sample weights of the pycnometer at 20.0 6 0.1C.4 Available from ASTM International Headquarters.5 Available from U.
27、S. Government Printing Office, Superintendent of Documents, 732 N. Capitol St., NW, Washington, DC 20401-0001, http:/www.access.gpo.gov.6 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed byth
28、e American Chemical Society, see Analar Standards for Laboratory Chemicals, VWR International BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.7 ASTM Manual on Presentation of Data and Control Chart Ana
29、lysis, 7th Edition, ASTM Manual Series MNL 7A (revision of Special Technical Publication (STP)15D).STP 15D.E202 1827. Report7.1 Report the relative density at 20/20C (in air) to the nearest 0.0001 unit.8. Precision and Bias8.1 The following criteria should be used for judging the acceptability of re
30、sults (see Note 1):8.1.1 Repeatability (Single Analyst)The standard deviation for a single determination has been estimated to be 0.0000651 unitat 96 dF. The 95 % limit for the difference between two such runs is 0.0002 unit.8.1.2 Laboratory Precision (Within-Laboratory, Between-Days)The standard de
31、viation of results (each the average ofduplicates), obtained by the same analyst on different days, has been estimated to be 0.0000598 units at 48 df. The 95 % limit forthe difference between two such averages is 0.0002 unit.8.1.3 Reproducibility (Multilaboratory)The standard deviation of results (e
32、ach the average of duplicates), obtained byanalysts in different laboratories, has been estimated to be 0.000191 unit at 5 dF. The 95 % limit for the difference between twosuch averages is 0.0005 unit.NOTE 1These precision estimates are based on interlaboratory studies performed in 1962 and 1963 on
33、six samples of the five glycols whose specificgravity values range from approximately 1.0233 to 1.1255.Atotal of ten laboratories cooperated in the studies in which each analyst performed duplicatedeterminations on each sample on each of two days.8 Practice E180 was used in developing these precisio
34、n estimates.8.2 BiasThe bias of this test method has not been determined due to the unavailability of suitable reference materials.9. Quality Guidelines9.1 Laboratories shall have a quality control system in place.9.1.1 Confirm the performance of the test instrument or test method by analyzing a qua
35、lity control sample following theguidelines of standard statistical quality control practices.9.1.2 A quality control sample is a stable material isolated from the production process and representative of the sample beinganalyzed.9.1.3 When QA/QC protocols are already established in the testing faci
36、lity, these protocols are acceptable when they confirmthe validity of test results.9.1.4 When there are no QA/QC protocols established in the testing facility, use the guidelines described in Guide D6809 orsimilar statistical quality control practices.DISTILLATION RANGE10. Procedure10.1 Determine th
37、e distillation range of the sample in accordance with Test Method D1078. Use the conditions as specified inTest Method D1078, and the ASTM Solvents Distillation Thermometer shown in Table 1 of Test Method D1078. (See Note 2 forcertain allowable exceptions in applying this test method to triethylene
38、glycol.)NOTE 2In the distillation of triethylene glycol, it may not be possible to collect the first drop of liquid within 15 min or to maintain the prescribeddistillation rate of 4 to 5 mL/min with some sources of gas. In this case, up to 30 min can be allowed to collect the first drop, and a disti
39、llation rate of2 to 3 mL/min is satisfactory. Alternatively, the flask chamber may be covered with a suitable shield so that only the upper neck and thermometer areexposed to room air to achieve the specified rates.10.2 Use the following values of K in the equation for barometric correction (Test Me
40、thod D1078):8 Supporting data have been filed at ASTM Headquarters and mymay be obtained by requesting Research Report:Report RR:E15-0013. Contact ASTM Customer Serviceat serviceastm.org.TABLE 1 Guide E2409 Glycol Impurities by Gas Chromatography (GC)Test Result,mg/kg SampleAverageover allLaboratori
41、esRepeatabilityStandardDeviationIntermediateStandardDeviationReproducibilityStandardDeviationRepeatabilityLimitIntermediateLimitReproducibilityLimitDEG MEG 374.59 7.3 7.3 34.0 20.6 20.6 95.3MEG DEG 1479.73 46.3 76.0 215.1 129.7 212.9 602.4TEG DEG 3499.69 92.8 143.2 306.5 260.0 401.0 858.3DEG TEG 489
42、.32 56.8 70.9 201.7 159.1 198.5 564.9TTEG TEG 1020.00 96.3 96.3 244.1 269.8 269.8 683.5DEG TeEG 1646.25 55.4 55.4 95.4 155.1 155.1 267.1TEG TeEG 7908.35 221.9 221.9 1350.7 621.2 621.2 3782.0PentaEG TeEG 2084.93 58.7 72.9 156.3 164.5 204.1 437.5E202 183Chemical KEthylene glycol 0.045Diethylene glycol
43、 0.050Triethylene glycol 0.055Propylene glycol 0.043Dipropylene glycol 0.05111. Report11.1 Report the corrected temperatures to the nearest 0.1C at each volume required by the specification for the glycol beinganalyzed.12. Precision and Bias12.1 Interlaboratory Study: 9, 1012.2 The precision of this
44、 test method was obtained from an interlaboratory study conducted in 2000 involving manual andautomatic distillation procedures. The study involved six samples of different boiling point ranges, done in duplicate. Tenlaboratories performed automatic Test Method D1078 distillation, and five laborator
45、ies performed manual Test Method D1078distillation. It was found that the precision is dependent on the boiling point temperature.The data were statistically evaluated usingASTM D2PP software (ASTM Adjunct ADJD6300).412.3 RepeatabilityTwo results, each the mean of two runs, obtained by the same oper
46、ator should be considered suspect if theydiffer by more than the repeatability values shown in Table 1 at a 95 % confidence level.12.4 ReproducibilityTwo results, each the mean of two runs, obtained by operators in different laboratories should beconsidered suspect if they differ by more than the re
47、producibility values shown in Table 1 at a 95 % confidence level.12.5 Bias:12.5.1 Absolute BiasSince the temperature measuring devices specified by this test method are calibrated against the normalboiling point of toluene (99.9+ % purity), this test method has no bias with respect to pure toluene a
48、s a reference material.12.5.2 Relative Bias Between Manual and Automatic D1078D1078 DistillationStatistical comparison between the variancesof automatic and manual D1078 distillation results did not indicate any statistically significant difference. Statistical comparisonof the averages of the six s
49、amples used in the study indicated that the paired-sample, two-tailed, t-test for the initial boiling point(IBP) and 50 % distillation point showed a small relative bias that is not statistically significant.Asmall but statistically significantbias was indicated for the automatic and manual D1078 dry point (DP). The observed bias (if any) are only for the samples studiedand may not be necessarily applicable to other samples.NOTE 3In cases of dispute, the parties involved may agree to designate either the manual or the automatic method
