ASTM D1177-2017 Standard Test Method for Freezing Point of Aqueous Engine Coolants《发动机冷却液冰点的标准试验方法》.pdf

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1、Designation: D1177 16D1177 17Standard Test Method forFreezing Point of Aqueous Engine Coolants1This standard is issued under the fixed designation D1177; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A

2、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 This test method covers the determination of the

3、 freezing point of an aqueous engine coolant solution in the laboratory.NOTE 1Where solutions of specific concentrations are to be tested, they shall be prepared from representative samples as directed in Practice D1176.Secondary phases separating on dilution need not be separated.NOTE 2These produc

4、ts may also be marketed in a ready-to-use form (prediluted).1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is

5、the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.1.4 This international standard was developed in accordance with internationally recognized principles on standardizationestablish

6、ed in the Decision on Principles 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:2D1176 Practice for Sampling and Preparing Aqueous Solutions of Engi

7、ne Coolants or Antirusts for Testing PurposesE1 Specification for ASTM Liquid-in-Glass Thermometers3. Terminology3.1 Definitions:3.1.1 freezing pointthe temperature at which crystallization begins in the absence of supercooling, or the maximumtemperature reached immediately after initial crystal for

8、mation in the case of supercooling, or the temperature at which solidcrystals, formed on cooling, disappear when the temperature of the specimen is allowed to rise.4. Summary of Test Method4.1 This test method involves the determination of the time-temperature curve prior to freezing and the determi

9、nation of thehorizontal or flattened portion of the freezing curve. The freezing point is taken as the intersection of projections of the coolingcurve and the freezing curve. If the solution supercools, the freezing point is the maximum temperature reached after supercooling.5. Significance and Use5

10、.1 The freezing point of an engine coolant indicates the coolant freeze protection.5.2 The freezing point of an engine coolant may be used to determine the approximate glycol content, provided the glycol typeis known.6. Apparatus6.1 Freezing Point Apparatus, shown assembled in Fig. 1, consisting of

11、the following:1 This test method is under the jurisdiction of ASTM Committee D15 on Engine Coolants and Related Fluids and is the direct responsibility of Subcommittee D15.03 onPhysical Properties.Current edition approved April 1, 2016April 1, 2017. Published May 2016April 2017. Originally approved

12、in 1951. Last previous edition approved in 20122016 asD1177 12.D1177-16. DOI: 10.1520/D1177-16.10.1520/D1177-17.2 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 s

13、tandardsstandards Document Summary page on the ASTM website.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 chan

14、ges 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, 100 Bar

15、r Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16.1.1 Cooling Bath, in which the refrigerant is contained, consisting of a standard 1.9-L (2-qt) Dewar flask. The flask may besilvered or unsilvered, and is supported in a close-fitting container.Apad of glass wool is place

16、d in the bottom of the flask to protectit from damage by tip of freezing tube.6.1.2 Freezing Tube3 consisting of a 200-mL(6.8-oz.)(6.8-oz) unevacuated, unsilvered Dewar flask. The tube is closed by a corkhaving a central hole for the thermocouple or resistance thermometer, a second hole placed to on

17、e side for passage of the stirringrod, and a third hole for introducing wire for seeding at appropriate time.6.1.3 Stirring Mechanism, consisting of a five-coil stirrer formed of stainless steel wire 1.6 mm (116 in.) in diameter. The coilsare so spaced that, in the extreme upward position during ope

18、ration, no coils are exposed above the surface of the sample. Thestirrer is agitated by means of an ordinary windshield wiper motor or other motor devices, operating through suitable linkages soas to provide linear motion of the stirrer. The length of the stroke is adjusted so that the coil just cle

19、ars the bottom of thefreezing-point tube at low point of the stroke.6.1.4 Temperature MeasurementA resistance thermometer or a multi-junction copper-constantan thermocouple may be usedwith suitable measuring instruments, providing these give an over-all sensitivity of 0.1C (0.2F).0.1 C (0.2 F). The

20、instrumentshall be calibrated before each series of determinations by using suitable reference standards. Platinum resistance thermometershave been adopted as a standard by the National Institute of Standards and Technology (NIST) and are recommended for thisstandard.NOTE 3ASTM Coolant Freezing Poin

21、t Temperature Measuring Instruments having a range from 37 to + 2C (35 to + 35F) or 54 to 15C(65 to + 5F)from 37 to +2 C (35 to +35 F) or 54 to 15 C (65 to +5 F) and conforming to the requirements for Thermometers 75F or 76F asprescribed in Specification E1, may be used where less accuracy is accept

22、able provided reference standards are used for calibration purposes.3 For routine work, a tube with a seeding tip as described in the paper by R. E. Mallonee and F. L. Howard, “The Determination of Freezing Point of Engine Antifreeze,”in the February 1951 issue of the ASTM Bulletin may be used.FIG.

23、1 Assembly of Freezing Point ApparatusD1177 1727. Refrigerant7.1 The refrigerant shall consist of solid carbon dioxide in alcohol or in other suitable bath liquids.NOTE 4A layer of dry ice, at least 13 mm (12 in.) thick, must be maintained in the bottom or on the top of the cooling bath during a det

24、ermination,depending on the bath liquid used. Adequate precautions should be taken against fire hazards or toxic effects of bath liquids, or both.7.2 Liquid nitrogen may be used as the refrigerant when the freezing point of the coolant is 46C (50F)is 46 C (50 F)or lower. (WarningThe liquid nitrogen

25、should be discarded after each daysdays use to avoid the possibility of explosion dueto dissolved oxygen and inadvertent mixing with organic coolant materials.)8. Procedure8.1 Assemble the apparatus as shown in Fig. 1, with no refrigerant and no sample of coolant yet in place. Check the operationof

26、the stirring mechanism after assembly to be sure that all parts operate freely.8.2 Fill the Dewar flask surrounding the freezing tube with the refrigerant liquid, adding pieces of solid carbon dioxide fromtime to time to maintain conditions mentioned in Note 4. Temporarily remove the stopper from th

27、e freezing tube and introduce75 to 100150 mL (2.65 to 3.4 oz.)5.1 oz) of the sample.NOTE 5The sample may be precooled to approximately 8C (15F)8 C (15 F) above the expected freezing point before introducing it into thefreezing tube.8.3 Start the stirrer and adjust it to operate at 60 to 80 strokes p

28、er min (Note 6).As soon as stirring is begun, observe and recordthe temperature at regular intervals of time. Electronic data acquisition systems may also be used in place of manual observationand recording. As the expected freezing point is approached, the time intervals shall be 10 to 15 s. At the

29、 expected freezing point,seeding shall be started to prevent supercooling. This shall be accomplished by introducing a wire which has a small portion ofthe solution being tested frozen on its tip. It is convenient to freeze this solution in a small test tube inserted directly into the coolingbath. T

30、he cooling rate shall be less than 1C (2F)/min1 C (2 F)min at the time the solution is seeded.NOTE 6A stroke is considered as a complete cycle of one upward and one downward motion of the stirrer.8.4 Continue temperature readings at regular intervals for at least 105 min after the apparent freezing

31、point.9. Report9.1 Report the following information:9.1.1 If the temperature-measuring instrument does not automatically plot temperature versus time, manually plot the observedtemperature against time on rectangular coordinate paper. time. Where the curve shows a definite flat or plateau during fre

32、ezing,the freezing point is taken as the intersection of projections of the cooling curve and the flat or horizontal plateau portion of thefreezing curve (see Fig. 2(a). If the solution supercools, the freezing point is the maximum temperature reached immediately aftersupercooling (see Fig. 2(b).NOT

33、E 7The amount of supercooling should be held to a minimum. If the supercooling exceeds 1C (2F)1 C (2 F) the test should be rejected.10. Precision and Bias10.1 Precision and Bias results are as follows:4C FRepeatability of Test for a Given Analyst 0.17 0.314 Supporting data have been filed at ASTM In

34、ternational Headquarters and may be obtained by requesting Research Report RR:D15-1010. Contact ASTM CustomerService at serviceastm.org.FIG. 2 Time-Temperature Cooling Curves for Determining the Freezing Point of an Engine CoolantD1177 173Intermediate Precision of Test for a Given Laboratory 0.88 1.

35、58Reproducibility of Test Across Laboratories 1.30 2.3411. Keywords11.1 aqueous engine coolants; engine coolants; engine coolants; freezing pointSUMMARY OF CHANGESSubcommittee D15.03 has identified the location of the selected changes to this standard since the last issue(D1177-12)-16) that may impa

36、ct the use of this standard.(1) The wordSection 8 “resistance” was added before “thermometer” inwas updated to reflect the volumes 6.1.2.in the onlycommercially available glassware at time of update.D1177 174(2) Mandatory languageSection 9 was added inupdated to 8.3.allow the use of digital plotting

37、. It previously read “manually plotthe observed temperature against time on rectangular coordinate paper.”(3) Note 7, which contains mandatory language, was deleted and the sentence was moved to 8.3.(4) The first sentence of 9.1.1 was revised.ASTM International takes no position respecting the valid

38、ity 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 standard is subje

39、ct 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 International Headquarte

40、rs. 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 below.This standard

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