ASTM D5949-2014 0677 Standard Test Method for Pour Point of Petroleum Products &40 Automatic Pressure Pulsing Method&41 《石油产品倾点40 自动压力脉冲法41的自动标准试验方法》.pdf

上传人:wealthynice100 文档编号:521104 上传时间:2018-12-03 格式:PDF 页数:6 大小:207.16KB
下载 相关 举报
ASTM D5949-2014 0677 Standard Test Method for Pour Point of Petroleum Products &40 Automatic Pressure Pulsing Method&41 《石油产品倾点40 自动压力脉冲法41的自动标准试验方法》.pdf_第1页
第1页 / 共6页
ASTM D5949-2014 0677 Standard Test Method for Pour Point of Petroleum Products &40 Automatic Pressure Pulsing Method&41 《石油产品倾点40 自动压力脉冲法41的自动标准试验方法》.pdf_第2页
第2页 / 共6页
ASTM D5949-2014 0677 Standard Test Method for Pour Point of Petroleum Products &40 Automatic Pressure Pulsing Method&41 《石油产品倾点40 自动压力脉冲法41的自动标准试验方法》.pdf_第3页
第3页 / 共6页
ASTM D5949-2014 0677 Standard Test Method for Pour Point of Petroleum Products &40 Automatic Pressure Pulsing Method&41 《石油产品倾点40 自动压力脉冲法41的自动标准试验方法》.pdf_第4页
第4页 / 共6页
ASTM D5949-2014 0677 Standard Test Method for Pour Point of Petroleum Products &40 Automatic Pressure Pulsing Method&41 《石油产品倾点40 自动压力脉冲法41的自动标准试验方法》.pdf_第5页
第5页 / 共6页
亲,该文档总共6页,到这儿已超出免费预览范围,如果喜欢就下载吧!
资源描述

1、Designation: D5949 14Standard Test Method forPour Point of Petroleum Products (Automatic PressurePulsing Method)1This standard is issued under the fixed designation D5949; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of

2、 last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.INTRODUCTIONThis test method covers an alternative procedure for the determination of pour point of petroleumproducts using an au

3、tomatic apparatus.1. Scope*1.1 This test method covers the determination of pour pointof petroleum products by an automatic instrument that appliesa controlled burst of nitrogen gas onto the specimen surfacewhile the specimen is being cooled and detects movement ofthe surface of the test specimen wi

4、th an optical device.1.2 This test method is designed to cover the range oftemperatures from 57 C to +51 C. However, the range oftemperatures included in the 1992 interlaboratory test programonly covered the temperature range from 39 C to +6 C andthe range of temperatures included in the 1998 interl

5、aboratorytest program was from 51 C to 11 C. (see 13.4).1.3 Test results from this test method can be determined at1 C or 3 C testing intervals.1.4 This test method is not intended for use with crude oils.NOTE 1The applicability of this test method or residual fuel sampleshas not been verified. For

6、further information on applicability, refer to13.4.1.5 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.6 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibi

7、lity 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:2D97 Test Method for Pour Point of Petroleum ProductsD4057 Practice for Manual Sampling of Petrole

8、um andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum Products2.2 Energy Institute Standard:IP 15 Test Method for Pour Point of Petroleum Products33. Terminology3.1 Definitions:3.1.1 pour point, nin petroleum products, the lowesttemperature at which movement of the

9、test specimen isobserved under the prescribed conditions of the test.3.2 Definitions of Terms Specific to This Standard:3.2.1 no-flow point, nin petroleum products, the tempera-ture of the test specimen at which a wax crystal structure orviscosity increase, or both, impedes movement of the surfaceof

10、 the test specimen under the conditions of the test.3.2.1.1 DiscussionThe no-flow point occurs when, uponcooling, the formation of wax crystal structures or viscosityincrease, or both, has progressed to the point where the appliedobservation device no longer detects movement under theconditions of t

11、he test. The preceding observation temperature,at which flow of the test specimen is last observed, is the pourpoint.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.07 on Flow Pro

12、perties.Current edition approved May 1, 2014. Published May 2014. Originallyapproved in 1996. Last previous edition approved in 2010 as D5949 10. DOI:10.1520/D5949-14.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual

13、Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,U.K., http:/www.energyinst.org.uk.*A Summary of Changes section appears at the end of this standardCopyright ASTM Internat

14、ional, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.2.2 pulse, na controlled burst of nitrogen gas of a fixedpressure and flow rate sufficient to cause movement on thesurface of the test specimen without fracturing the waxstructure which may be formed in the

15、specimen.3.2.3 Peltier device, na solid-state thermoelectric deviceconstructed with dissimilar semiconductor materials, config-ured in such a way that it will transport heat to or away froma test specimen dependent on the direction of electric currentapplied to the device.4. Summary of Test Method4.

16、1 After inserting the test specimen into the automatic pourpoint apparatus, and initiation of the test program, the testspecimen is heated and then cooled by a Peltier device at a rateof 1.5 C/min 6 0.1 C/min. At temperature intervals of 1 Cor 3 C, depending on the selection made by the user, a movi

17、ngforce in the form of a pressurized pulse of nitrogen gas isimparted onto the surface of the specimen. Multiple opticaldetectors are used in conjunction with a light source to monitormovement of the surface of the specimen. The lowest tempera-ture at which movement of the specimen surface is observ

18、edupon application of a pulse of nitrogen gas is recorded as thepour point, Test Method D5949.5. Significance and Use5.1 The pour point of a petroleum product is an index of thelowest temperature of its utility for certain applications. Flowcharacteristics, like pour point, can be critical for the c

19、orrectoperation of lubricating oil systems, fuel systems, and pipelineoperations.5.2 Petroleum blending operations require precise measure-ment of the pour point.5.3 In most cases, this test method does not require the useof mechanical refrigeration apparatus (see 7.1).5.4 This test method yields a

20、pour point in a format similarto Test Method D97/IP 15 when the 3 C interval results arereported.NOTE 2Since some users may wish to report their results in a formatsimilar to Test Method D97 (in 3 C intervals) the precisions were derivedfrom the temperatures rounded to the 3 intervals. For statement

21、s on biasrelative to Test Method D97, see 13.3.5.5 Test results from this test method can be determined ateither 1 C or 3 C intervals.5.6 This test method has better repeatability and reproduc-ibility relative to Test Method D97/IP 15 as measured in the1992 and 1998 interlaboratory test programs.46.

22、 Apparatus6.1 Automatic Apparatus5The automatic pour point appa-ratus described in this test method consists of a microprocessorcontrolled test chamber that is capable of heating and coolingthe test specimen, providing a controlled pulse of nitrogen gasonto the specimen surface, optically detecting

23、the specimensurface movement, and recording the temperature of thespecimen as described in detail in Annex A1. It is specificallydesigned to detect the lowest temperature at which movementof the surface of the specimen is observed upon application ofthe pulse.6.2 The apparatus shall be equipped with

24、 a specimen cup, anarray of optical detectors, light source, pressure pulsing unit,digital display, Peltier device, and a specimen temperaturemeasuring device.6.3 The pressure pulsing unit consists of a stainless steeltubing, 250 mm 6 2 mm long and 1.1 mm 6 0.1 mm insidediameter. This tubing is conn

25、ected to a constant pressuresource at one end, which serves as an inlet.The other end of thetubing, which serves as the outlet, is bent and positioned suchthat it is pointing to the center of the specimen at an acuteangle. The distance between the outlet and the center of thespecimen is 8 mm 6 2 mm.

26、6.4 The Peltier device shall be capable of heating or coolingthe test specimen at a rate of 1.5 C/min 6 0.1 C/min.6.5 The temperature measuring device in the specimen cupshall be capable of measuring the temperature of the testspecimen from 80 C to +70 C at a resolution of 0.1 C.6.6 The apparatus sh

27、all be equipped with fittings to permitthe circulation of water or other liquid cooling media to removeheat generated by the Peltier device and other electroniccomponents of the apparatus.6.7 The apparatus shall be equipped with fittings to permitthe delivery of nitrogen gas to the pressure pulsing

28、unit.6.8 Ultrasonic Bath, Unheated(optional)with an oper-ating frequency between 25 kHz to 60 kHz and a typical poweroutput of 100 W, of suitable dimensions to hold container(s)placed inside of bath, for use in effectively dissipating andremoving air or gas bubbles that can be entrained in viscous4T

29、he results of this interlaboratory test program are available from ASTMInternational Headquarters in the form of a research report. Request RR:D02-1312for the 1992 program and RR:D02-1499 for the 1998 program.5The following instrument has been found suitable for use in this test method:Phase Technol

30、ogy Pour Point Analyzer model series 30, 50, 70, 70V and 70X;available from Phase Technology, 11168 Hammersmith Gate, Richmond, B.C.CanadaV7A5H8. In the 1998 research report, the 70Vwas referred to as the currentmodel; whereas models 30, 50, and 70 were referred to as pre-1998 models. Thevarious mod

31、el series mentioned above are differentiated by their cooling capacitiesand user interfaces; however, all of them are capable of covering the entiretemperature range specified in the scope.This pour point analyzer is covered by a patent. Interested parties are invited tosubmit information regarding

32、the identification of an alternative to this patented itemto the ASTM International Headquarters. Your comments will receive carefulconsideration at a meeting of the responsible technical committee which you mayattend.D5949 142sample types prior to analysis. It is permissible to use ultra-sonic bath

33、s with operating frequencies and power outputsoutside this range, however it is the responsibility of thelaboratory to conduct a data comparison study to confirm thatresults determined with and without the use of such ultrasonicbaths does not materially impact results.7. Reagents and Materials7.1 Co

34、olantTap water or other liquid heat exchange me-dium sufficient to remove heat generated by the Peltier deviceand other electronic components from the apparatus. Toachieve specimen cooling to 60 C, supply circulation ofliquid cooling medium at +25 C or lower to the apparatus.Obtain cooling performan

35、ce data from the apparatus manufac-turer if lower specimen temperatures are desired or if the tapwater temperature is higher than 25 C.7.2 Dry Nitrogen GasNitrogen gas with a dew pointbelow the lowest temperature attained by the specimen(WarningCompressed gas.)(WarningInert gas can be anasphyxiant w

36、hen inhaled.)7.3 Precision Volume-Dispensing Device, capable of dis-pensing 0.150 mL 6 0.005 mL of sample.7.4 Cotton Swab, plastic shaft cotton swabs to clean thesample cup.8. Sampling8.1 Obtain a sample in accordance with Practice D4057 orby Practice D4177.8.2 Samples of very viscous materials may

37、be warmed untilthey are reasonably fluid before they are transferred; however,no sample shall be heated more than is absolutely necessary.The sample shall not be heated and transferred into the testspecimen cup unless its temperature is 70 C or lower.NOTE 3In the event the sample has been heated abo

38、ve thistemperature, allow the sample to cool until its temperature is at least 70 Cbefore transferring.8.3 For some sample types, such as viscous lube oils that areprone to having entrained air or gas bubbles present in thesample, the use of an ultrasonic bath (see 6.8) without theheater turned on (

39、if so equipped), has been found effective indissipating bubbles typically within 1 min.9. Preparation of Apparatus9.1 Install the analyzer for operation in accordance with themanufacturers instructions.9.2 Turn on the liquid cooling medium and ensure itstemperature is appropriate for the specimen be

40、ing tested inaccordance with manufacturers instructions (see 7.1).9.3 Turn on the nitrogen gas and ensure that it is regulatedto the appropriate pressure in accordance with the manufactur-ers instructions.9.4 Turn on the main power switch of the analyzer.10. Calibration and Standardization10.1 Ensur

41、e that all of the manufacturers instructions forcalibrating, checking, and operating the apparatus are fol-lowed.10.2 A sample with a well-documented pour point can beused to verify performance of the apparatus. Alternatively, asample which has been extensively tested in a pour pointinterlaboratory

42、study can be used.11. Procedure11.1 Inspect the specimen cup to ensure that it is clean anddry. If needed, clean the cup in accordance with 11.3.11.2 Deliver 0.150 mL 6 0.005 mL of specimen into thespecimen cup. Pipettes, syringes, or precision positive-displacement devices are suitable for use in d

43、elivering thespecimen. Samples with an expected pour point above 36 C orwhich appear solid at room temperature may be heated above45 C, but shall not be heated above 70 C (see Note 4).11.3 Clean the specimen out of the cup. The cup shall becleaned to the point where no visible droplets of specimenre

44、main in the cup. Non-abrasive absorbent materials, such ascotton swabs, are suitable for use in cleaning the specimen cup.Cleaning solvents able to clean the specimen and compatiblewith the components of the apparatus may also be used.Naphtha, hexane, and heptane are suitable as cleaning solvents.11

45、.4 Repeat steps 11.2 and 11.3.11.5 Carefully measure 0.150 mL 6 0.005 mL of thespecimen into the specimen cup.11.6 Close and lock the test chamber lid.11.7 Follow the manufacturers instructions for preheatingthe specimen.11.8 Select the desired pour point testing interval: 1 C or3 C.11.9 Start the t

46、est program following the manufacturersinstructions. The specimen is first heated as specified in 11.7.Itis then cooled by the Peltier device at a rate of 1.5 C/min 60.1 C/min. The apparatus will apply a pulse of pressurizednitrogen gas onto the specimen surface every 1 C or 3 C dropin temperature d

47、epending on the testing interval specified in11.8. The specimen is illuminated by the light source, and themovement of the specimen surface upon application of a pulseis monitored by an array of optical detectors. The test willcontinue until application of a pulse of nitrogen gas causes noobservable

48、 movement on the specimen surface. This is theno-flow point of the specimen. The lowest temperature atwhich movement of the specimen surface is observed uponapplication of the pulse of nitrogen gas is recorded as the pourpoint. The pour point value shall be displayed as an integertemperature in mult

49、iples of 1 C or 3 C depending on theselected testing interval.11.10 Open the test chamber lid to access the specimen cupand clean the specimen out of the specimen cup (see 11.3).12. Report12.1 Report the temperature recorded in 11.9 together withthe testing interval as pour point Test Method D5949.13. Precision and Bias13.1 PrecisionThe precision of this test method as deter-mined by the statistical examination of the interlaboratory testresults4is as follows:D5949 14313.1.1 RepeatabilityThe difference between su

展开阅读全文
相关资源
猜你喜欢
相关搜索

当前位置:首页 > 标准规范 > 国际标准 > ASTM

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