1、Designation:E20210 Designation: E202 12Standard 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 o
2、f last revision. 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 Department of Defense.1. Scope*1.1 These test methods cover the chemi
3、cal and 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 9-11Acidity 12-14Water 15-1
4、7Iron 18-20Color 21-23Gas Chromatographic Analysis 24-26Alternative Test Methods AppendixX11.2 Review the current appropriate Material Safety Data Sheets (MSDS) for detailed information concerning toxicity, first aidprocedures, and safety precautions.1.3 The values stated in SI units are to be regar
5、ded as standard. No other units of measurement are included in this standardwith the exception of foot-pound for apparatus descriptions.1.4 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 e
6、stablish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D891 Test Methods for Specific Gravity, Apparent, of Liquid Industrial ChemicalsD1078 Test Method for Distillation Range of Volatile Organ
7、ic LiquidsD1193 Specification for Reagent WaterD1209 Test Method for Color of Clear Liquids (Platinum-Cobalt Scale)D1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lacquer, and RelatedProductsD4052 Test Method for Density, Relative Density, and AP
8、I Gravity of Liquids by Digital Density MeterD5386 Test Method for Color of Liquids Using Tristimulus ColorimetryE180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty ChemicalsE203 Test Method for Water Using Volumetric Karl Fischer Titratio
9、nE394 Test Method for Iron in Trace Quantities Using the 1,10-Phenanthroline MethodE611 Test Methods for Low Concentrations of Diethlyene Glycol in Ethylene Glycol by Gas ChromatographyE1064 Test Method for Water in Organic Liquids by Coulometric Karl Fischer TitrationE1615 Test Method for Iron in T
10、race Quantities Using the FerroZine MethodE2409 Test Method for Glycol Impurities in Mono-, Di-, Tri- and Tetraethylene Glycol (Gas Chromatographic Method)E2679 Test Method for Acidity in Mono-, Di-, Tri- and Tetraethylene Glycol byNon-Aqueous Potentiometric Titration1These test methods are under th
11、e jurisdiction of ASTM Committee E15 on Industrial and Specialty Chemicals and are the direct responsibility of Subcommittee E15.01on General Standards.Current edition approved Aug.April 1, 2010.2012. Published September 2010.May 2012. Originally approved in 1962. Last previous edition approved in 2
12、0092010 asE20209.E20210. DOI: 10.1520/E0202-102.2For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.1This docum
13、ent 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 changes accurately, ASTM recommends that users consult prior editions as a
14、ppropriate. 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 standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United
15、 States.2.2 ASTM Adjuncts:Adjunct ADJD6300 Determination of Precision and Bias for Use in Test Methods for Petroleum Products and Lubricants33. Significance and Use3.1 These test methods measure certain chemical and physical properties of ethylene glycols and propylene glycols and maybe used to dete
16、rmine compliance with specification in which limits are established for these properties. For those tests that use theprocedure of another ASTM test method, that test method should be consulted for additional information on the significance anduse of that test.3.2 Alternative test methods and techno
17、logy for several of the methods can be found in the Appendix. Use of these methodsis optional and individuals using the alternative methods should assure themselves that the method is sufficient and appropriate forthe application. Precision data presented in this standard is only for the original te
18、st methods listed.4. Purity of Reagents4.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, wheresuch specifi
19、cations are available.4Other grades may be used, provided it is first ascertained that the reagent is of sufficiently highpurity to permit its use without lessening the accuracy of the determination.4.2 Unless otherwise indicated, references to water shall be understood to mean reagent water conform
20、ing to SpecificationD1193, Type II or III.5. Quality Control5.1 It is recommended that a control chart for the concentration of the impurities in the glycol quality control sample beestablished and maintained according to common guidelines.5Measure the control sample each time a test sample(s) is te
21、sted. Ifthe measured value exceeds the action limit of the control chart, take appropriate action before proceeding with sample tests.SPECIFIC GRAVITY6. Procedure6.1 Determine the relative density of the sample at 20/20C using the pycnometer test method in accordance with Test MethodsD891, except de
22、termine the water and sample weights of the pycnometer at 20.0 6 0.1C.7. 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 results (see Note 1):8.1.1 Repeatability (Singl
23、e Analyst)The standard deviation for a single determination has been estimated to be 0.0000651unit at 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 deviation of results (each the average ofduplic
24、ates), 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 (each the average of duplicates), obtained bya
25、nalysts 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 six samples of the five glycols whose specif
26、icgravity values range from approximately 1.0233 to 1.1255. A total of ten laboratories cooperated in the studies in which each analyst performed duplicatedeterminations on each sample on each of two days.6Practice E180 was used in developing these precision estimates.8.2 BiasThe bias of this test m
27、ethod has not been determined due to the unavailability of suitable reference materials.3Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards
28、 for Laboratory Chemicals, VWR International Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia andNational Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.3Available from ASTM International Headquarters.4ASTM Manual on Presentation of Data and Control Chart Analysis,
29、 7th Edition, ASTM Manual Series MNL 7A (revision of Special Technical Publication (STP) 15D).4Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Sta
30、ndards for Laboratory Chemicals, VWR International Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia andNational Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.5Supporting data have been filed at ASTM Headquarters and my be obtained by requesting Research Report RR:
31、 RR:E15-0013.5ASTM Manual on Presentation of Data and Control Chart Analysis, 7th Edition, ASTM Manual Series MNL 7A (revision of Special Technical Publication (STP) 15D).6Supporting data have been filed at ASTM Headquarters and my be obtained by requesting Research Report RR: RR:E15-1064. RR:E15-00
32、13.E202 122DISTILLATION RANGE9. Procedure9.1 Determine the 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 allowabl
33、e exceptions in applying this test method to triethylene 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
34、min can be allowed to collect the first drop, and a distillation 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.9.2 Use the following values
35、 of K in the equation for barometric correction (Test Method D1078):Chemical KEthylene glycol 0.045Diethylene glycol 0.050Triethylene glycol 0.055Propylene glycol 0.043Dipropylene glycol 0.05110. Report10.1 Report the corrected temperatures to the nearest 0.1C at each volume required by the specific
36、ation for the glycol beinganalyzed.11. Precision and Bias11.1The following criteria should be used for judging the acceptability of results (Note 3):11.1.1Repeatability (Single Analyst)The standard deviation for a single determination has been estimated to be the value inTable 2 of Test Method11.1 I
37、nterlaboratory Study:7,811.2 The precision of this 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
38、Test Method D1078 at the indicated degrees of freedom. The 95% limit for the differencebetween two such runs is the value in the table.11.1.2Laboratory Precision (Within-Laboratory, Between-Days)The standard deviation of results (each the average ofduplicates), obtained by the same analyst on differ
39、ent days, has been estimated to be the value in Table 1 at the indicated degreesof freedom. The 95% limit for the difference between two such averages is the value in the table.11.1.3Reproducibility (Multilaboratory) The standard deviation of results (each the average of duplicates), obtained byanal
40、ysts in different laboratories, has been estimated to be the value in Table 1 at the indicated degrees of freedom. The 95% limitfor the difference between two such averages is the value in the table. distillation, and five laboratories performed manual TestMethod D1078 distillation. It was found tha
41、t the precision is dependent on the boiling point temperature. The data were statisticallyevaluated using ASTM D2PP software (ASTM Adjunct ADJD6300).311.3 RepeatabilityTwo results, each the mean of two runs, obtained by the same operator should be considered suspect if theydiffer by more than the re
42、peatability values shown in Table 1 at a 95 % confidence level.7Supporting data have been filed at ASTM Headquarters and my be obtained by requesting Research Report RR:RR:E15-1063.RR: RR:E15-1114.8These Parameters are summarized in Table X2.1 as typical values. See Note X2.4.8Supporting data have b
43、een filed at ASTM Headquarters and my be obtained by requesting Research Report RR: RR:E15-1123.TABLE 1 Guide E2409 Glycol Impurities by Gas Chromatography (GC)Test Result,mg/kgSampleAverageover allLaboratoriesRepeatabilityStandardDeviationIntermediateStandardDeviationReproducibilityStandardDeviatio
44、nRepeatabilityLimitIntermediateLimitReproducibilityLimitDEG 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 489.32 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 T
45、eEG 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 12311.4 ReproducibilityTwo results, each the mean of two runs, obtained by operators in different laboratories should beconsidered suspect if t
46、hey differ by more than the reproducibility values shown in Table 1 at a 95 % confidence level.11.5 Bias:11.5.1 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
47、with respect to pure toluene as a reference material.11.5.2 Relative Bias Between Manual and Automatic D1078 DistillationStatistical comparison between the variances ofautomatic and manual D1078 distillation results did not indicate any statistically significant difference. Statistical comparison of
48、the averages of the six samples 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 auto
49、matic 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.NOTE3These precision estimates are based on interlaboratory studies performed in 1962 and 1963 on eleven samples of the five glycols whosedistillation ranges varied from 1.4 to 9.7C. A total of ten laboratories cooperated in the studies in which each analyst performed duplicate determinationson each sample on each of two days.5Practice E180 was used in developing these precision estimates.11.2BiasThe bias of
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