ImageVerifierCode 换一换
格式:PDF , 页数:5 ,大小:99.10KB ,
资源ID:519923      下载积分:10000 积分
快捷下载
登录下载
邮箱/手机:
温馨提示:
如需开发票,请勿充值!快捷下载时,用户名和密码都是您填写的邮箱或者手机号,方便查询和重复下载(系统自动生成)。
如填写123,账号就是123,密码也是123。
特别说明:
请自助下载,系统不会自动发送文件的哦; 如果您已付费,想二次下载,请登录后访问:我的下载记录
支付方式: 支付宝扫码支付 微信扫码支付   
注意:如需开发票,请勿充值!
验证码:   换一换

加入VIP,免费下载
 

温馨提示:由于个人手机设置不同,如果发现不能下载,请复制以下地址【http://www.mydoc123.com/d-519923.html】到电脑端继续下载(重复下载不扣费)。

已注册用户请登录:
账号:
密码:
验证码:   换一换
  忘记密码?
三方登录: 微信登录  

下载须知

1: 本站所有资源如无特殊说明,都需要本地电脑安装OFFICE2007和PDF阅读器。
2: 试题试卷类文档,如果标题没有明确说明有答案则都视为没有答案,请知晓。
3: 文件的所有权益归上传用户所有。
4. 未经权益所有人同意不得将文件中的内容挪作商业或盈利用途。
5. 本站仅提供交流平台,并不能对任何下载内容负责。
6. 下载文件中如有侵权或不适当内容,请与我们联系,我们立即纠正。
7. 本站不保证下载资源的准确性、安全性和完整性, 同时也不承担用户因使用这些下载资源对自己和他人造成任何形式的伤害或损失。

版权提示 | 免责声明

本文(ASTM D5483-2005(2010) Standard Test Method for Oxidation Induction Time of Lubricating Greases by Pressure Differential Scanning Calorimetry《用压差扫描热量测定法测试润滑脂的氧化反应时间的标准试验方法》.pdf)为本站会员(Iclinic170)主动上传,麦多课文库仅提供信息存储空间,仅对用户上传内容的表现方式做保护处理,对上载内容本身不做任何修改或编辑。 若此文所含内容侵犯了您的版权或隐私,请立即通知麦多课文库(发送邮件至master@mydoc123.com或直接QQ联系客服),我们立即给予删除!

ASTM D5483-2005(2010) Standard Test Method for Oxidation Induction Time of Lubricating Greases by Pressure Differential Scanning Calorimetry《用压差扫描热量测定法测试润滑脂的氧化反应时间的标准试验方法》.pdf

1、Designation: D5483 05 (Reapproved 2010)Standard Test Method forOxidation Induction Time of Lubricating Greases byPressure Differential Scanning Calorimetry1This standard is issued under the fixed designation D5483; the number immediately following the designation indicates the year oforiginal adopti

2、on or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of oxidationinduction time of lu

3、bricating greases subjected to oxygen at3.5 MPa (500 psig) and temperatures between 155 and 210C.1.2 The values stated in SI units are to be regarded asstandard. The values given in parentheses are for informationonly.1.3 This standard does not purport to address all of thesafety concerns, if any, a

4、ssociated with its use. 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:2E473 Terminology Relating to Thermal Analysis and Rhe-

5、ology3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 extrapolated onset time, na time determined on athermal curve, as the intersection of the extrapolated baselineand a line tangent to the oxidation exotherm constructed at itsmaximum rate.3.1.2 oxidation induction time (OIT),

6、 n the period of timefrom the first exposure to an oxidizing atmosphere until theextrapolated onset time.3.1.3 pressure differential scanning calorimeter, (PDSC),na differential scanning calorimeter, as defined in Terminol-ogy E473, that is capable of maintaining the test sample at acontrolled, elev

7、ated pressure.3.1.4 thermal curve, na graph of sample heat flow versustime.4. Summary of Test Method4.1 A small quantity of grease is weighed into a sample panand placed in a test cell. The cell is heated to a specifiedtemperature and then pressurized with oxygen. The cell is heldat a regulated temp

8、erature and pressure until an exothermicreaction occurs. The extrapolated onset time is measured andreported as the oxidation induction time for the grease underthe specified test temperature.4.2 A kinetic equation incorporated with this test methodcan estimate oxidation induction times at other tem

9、peratures.5. Significance and Use5.1 Oxidation induction time, as determined under theconditions of this test method, can be used as an indication ofoxidation stability.3This test method can be used for researchand development, quality control and specification purposes.However, no correlation has b

10、een determined between theresults of this test method and service performance.6. Apparatus6.1 Pressure Differential Scanning Calorimeter (PDSC),equipped with the following items (see Fig. 1).4NOTE 1At the time that the round robin data for this test method wasgenerated, only TA Instruments4manufactu

11、red equipment that met therequirements of 5.1. Subsequently, other companies have manufacturedequipment meeting these requirements. Their use is permitted providedtheir performance is consistent with the repeatability and reproducibilitydescribed in Section 10.6.1.1 Sample Enclosure, with capability

12、 to 3.5 MPa (500psig) at 210C and pressure gauge graduated at intervals of 200kPa (28.6 psi) or less.6.2 Thermal Analyzer.6.3 Aluminum Sample Solid Fat Index (SFI), pan (see Note2).6.4 Oxidation Stability Software.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products

13、 and Lubricants and is the direct responsibility of SubcommitteeD02.09.0E on Oxidation of Greases.Current edition approved Oct. 1, 2010. Published November 2010. Originallyapproved in 1993. Last previous edition approved in 2005 as D548305. DOI:10.1520/D5483-05R10.2For referenced ASTM standards, vis

14、it the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Rhee, In-Sik, “Development of a New Oxidation Stability Test Method forGreases Using a Pressure

15、 Differential Scanning Calorimeter (PDSC),” NLGISpokesman, Vol 55, No. 4, July 1991, pp. 123132.4The sole source of supply of the apparatus known to the committee at this timeis TA Instruments, Inc., 109 Lukens Drive, New Castle, DE 19720. If you are awareof alternative suppliers, please provide thi

16、s information to ASTM InternationalHeadquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee,1which you may attend.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.5 Calibratio

17、n Software.6.6 Flowmeter, with a capacity of at least 200 mL/min.6.7 Sample Encapsulation Press.NOTE 2It has been found that grease samples can be prepared withmore consistent surface areas using SFI pans as compared to flat bottompans, resulting in better reproducibility.NOTE 3See Fig. 1 for a diag

18、ram of a typical test unit.7. Reagents and Materials7.1 Oxygen, extra dry, of not less than 99.5 % purity byvolume. (WarningOxidizer. Gas under pressure. In additionto other precautions, use stainless steel or copper tubing whichis compatible with oxygen, and pressure gauges which aredesignated for

19、use with oxygen.)7.2 Indium, of not less than 99.9 % purity by mass.8. Calibration8.1 Sample Temperature Calibration:8.1.1 Weigh approximately 10 mg of indium into an alumi-num sample pan, insert a lid and crimp the lid to the pan usingthe encapsulation press. Place the crimped pan onto the samplepl

20、atform in the pressure cell. Seal an empty pan in the samemanner and place it on the reference platform. Set the cellcover in place and close the cell.8.1.2 Open the oxygen cylinder valve slightly and set apressure of 3.5 6 0.2 MPa (500 6 25 psig) on the cell inlet linewith the pressure regulator. P

21、artially open the inlet valve on thecell and allow the pressure to slowly build up in the cell. Thisshould require approximately 2 min. Using the outlet valve,adjust the oxygen purge rate through the flowmeter to 100 610 mL/min. The open position of these valves should remainfixed during the test.8.

22、1.3 Set the thermal analyzer to heat from ambient tem-perature (approximately 22C) to 180C) at a programmed rateof 10C/min. After completion of the run, measure the meltingtemperature of the indium. If the melting temperature differsfrom 157.4 6 0.2C (see Note 4), correct the difference byusing eith

23、er the hardware or software calibration proceduredescribed in the manufacturers instruction manual. If thehardware calibration procedure is used, the temperature cor-rection should be performed under 3.5 MPa (500 psig) oxygenpressure with a 100 mL/min purge rate. A typical meltingcalibration curve i

24、s shown in Fig. 2.NOTE 4The melting temperature of indium is 156.6C at atmosphericpressure, but has been found to be elevated to 157.4C under theconditions of this test method, 3.5 MPa (500 psig) of oxygen.58.2 Temperature Controller Calibration:8.2.1 Remove both the sample pan and the reference pan

25、from the cell, then close the cell. Slowly pressurize the cellwith 3.5 6 0.2 MPa (500 6 25 psig) oxygen and adjust thepurge rate to 100 6 10 mL/min using the cell outlet valve.Select the desired test temperature (either 210, 180, or 155C).8.2.2 Program the cell to maintain the selected test tempera-

26、ture. If, after 10 min, the displayed cell temperature differs bymore than 60.2C from the selected temperature, slowly adjustthe temperature controller until they agree. After making anadjustment, wait at least 5 min to make certain that thetemperature is stable before continuing.8.2.3 Some of the n

27、ewest instruments do not need this stepdue to their automatic calibration system. Therefore, thecontrol thermocouple calibaration should be performed accord-ing to the instruments manual.8.3 Cell Base Pressure Gauge CalibrationThe calibrationshould be conducted using a calibrated pressure transducer

28、 ora previously calibrated gauge according to the pressure cellmanufacturers instructions.9. Procedure9.1 Before starting a test, the control thermocouple calibra-tion shall be conducted at the test temperature (either 210, 180,or 155C) according to 8.2.1 and 8.2.2. When the test tempera-ture is not

29、 known, the calibration should be conducted at210C. Ignore this step if the instrument already has anautomatic temperature controller calibration system.9.2 Weigh 2.0 6 0.1 mg of grease into a sample pan. Spreadthe sample evenly upon the flat portion. Do not spill any of thesample into the trough po

30、rtion of the pan (See Fig. 3).NOTE 5Examples of suitable and poor sample on pan patterns areshown in Fig. 3.9.3 Place the uncovered pan containing the sample onto theplatform of the cell according to the PDSC manufacturersinstructions for placing the sample pan. Place an empty pan ofthe same configu

31、ration onto the cell platform according to thePDSC manufacturers instructions for placing the referencepan. Close the cell and the pressure release valve.9.4 Beginning at ambient temperature (approximately22C), program the sample temperature to increase at a rate of100C/min to the test temperature.9

32、.5 Allow the sample to equilibrate at the test temperaturefor 2 min.NOTE 6This step did not appear in the test method which was used inthe round robin to generate the precision statement. The round robin testmethod used the software of a PDSC manufacturer to determine whenequilibration at test tempe

33、ratures occurred. Step 9.5 removes this depen-dence on one PDSC manufacturer and is not expected to significantlyaffect the measured OIT since this step precedes the pressurization of thetest cell with oxygen.5Supporting data have been filed at ASTM International Headquarters and maybe obtained by r

34、equesting Research Report RR:D02-1007.FIG. 1 PDSC Test UnitD5483 05 (2010)29.6 Open the oxygen valve and slowly pressurize the cell to3.5 6 0.2 MPa (500 6 25 psig). This should require approxi-mately 2 min to reach maximum pressure. The oxidationinduction time is measured from the time when the oxyg

35、envalve is opened.9.7 As soon as the pressure has equilibrated, check the cellpurge rate and adjust to 100 6 10 mL/min with the outletvalve.9.8 After a duration of 120 min from the time when theoxygen valve was opened, close the oxygen valve and slowlyrelease the cell pressure by opening the cell pr

36、essure releasevalve. In the case of a sample for which the approximateoxidation induction time is known, the test can be stopped afterthe oxidation exotherm has occurred.9.9 Plot the thermal curve and measure the extrapolatedonset time for the oxidation exotherm. Report this time, to thenearest tent

37、h of one minute, as the oxidation induction time forthe sample. If more than one oxidation exotherm is observed,record the oxidation induction time for the largest exotherm(See Fig. 4).NOTE 7A typical thermal curve is shown in Fig. 4.9.10 If the induction time is less than 10 min, rerun the testat t

38、he next lower temperature, starting at 9.2. Allow the cell tocool to ambient temperature before running the test at the nextlower temperature.9.11 After the oxidation induction time requirement speci-fied in 9.10 is satisfied, perform a duplicate test.9.12 If the difference between the two results i

39、s greater thanthe 95% determinability limit stated in the Precision and Biassection of this test method (Section 12), then reject the resultsand determine two more oxidation induction times for thegrease by returning to 9.2. Otherwise, average the oxidationinduction times of both runs.10. Calculatio

40、n of Induction Times for OtherTemperatures10.1 After an oxidation induction time has been determinedfor a particular grease, a value can be estimated for othertemperatures using the following equation:t 5 A exp 17 500/T! (1)where:t = estimated oxidation induction time, min,A = oxidation coefficient

41、of the grease, andT = temperature, K (for desired temperature).The oxidation coefficient (A) is constant for a given greaseand is calculated by (Eq 1) using the oxidation induction timereported in 9.1.2, thus,A 5 oxidation induction time/exp17 500/test temperature, K!.(2)The estimated oxidation indu

42、ction time can be used as aguide for choosing appropriate alternative test temperatures fora grease. The estimated oxidation induction time is not a partof the report for this test method.11. Report11.1 Report the following information:11.1.1 Report, to the nearest tenth of one minute, theaverage va

43、lue calculated in 9.12 as the oxidation inductiontime (OIT) for the sample.11.1.2 Report the test temperature.FIG. 2 CalibrationFIG. 3 Sample Preparation on SFI PanD5483 05 (2010)312. Precision and Bias612.1 The precision of this test method as determined by thestatistical examination of interlabora

44、tory test results involvingeleven samples, five laboratories, three test temperatures (155,180, and 210C), and oxidation induction times of from 9.0 to45.3 minutes is as follows.12.1.1 Determinability The difference between the pair ofdeterminations averaged to obtain a test result would, in thelong

45、 run, in the normal and correct operation of the testmethod, exceed the following value in only one case in twenty:Determinability 5 0.59=m (3)where:m = the mean of the two determinations12.1.2 Repeatability The difference between successiveresults (each the mean of a pair of determinations) obtaine

46、d bythe same operator with the same apparatus under constantoperating conditions on identical material, would in the longrun, in the normal and correct operation of the test method,exceed the following value in only one case in twenty:Repeatability 5 0.42=m (4)where:m = is the mean of the two result

47、s12.1.3 ReproducibilityThe difference between two inde-pendent results (each the mean of a pair of determinations)obtained by different operators working in different laborato-ries would, in the long run, exceed the following value onlyone case in twenty:Reproducibility 5 0.71=m (5)where:m = the mea

48、n of the two test results.12.2 BiasThe procedure in this test method has no biasbecause the value of oxidation induction time can be definedonly in terms of a test method.13. Keywords13.1 differential scanning calorimetry; lubricating grease;OIT; onset temperature; oxidation; oxidation coefficient;

49、oxi-dation induction time; PDSC; thermal analysis6Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D02-1314.FIG. 4 Typical PDSC Thermal CurveD5483 05 (2010)4APPENDIX(Nonmandatory Information)X1. PDSC ROUND ROBIN DATAX1.1 See Table X1.1 for PDSC Round Robin data.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 are expressly advised that determination of t

copyright@ 2008-2019 麦多课文库(www.mydoc123.com)网站版权所有
备案/许可证编号:苏ICP备17064731号-1