1、Designation:D734607 Designation: D7346 12Standard Test Method forNo Flow Point of Petroleum ProductsNo Flow Point andPour Point of Petroleum Products1This standard is issued under the fixed designation D7346; the number immediately following the designation indicates the year oforiginal adoption or,
2、 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. Scope1.1This test method covers the determination of the no flow point temperature of pet
3、roleum products using an automaticinstrument.1.2The measuring range of the apparatus is from -95 to 45C, however the precision statements were derived only from sampleswith no flow point temperatures from -77 to +2C.1.3The values stated in SI units are to be regarded as standard. No other units of m
4、easurement are included in this standard.1.41.1 This test method covers the determination of the no flow point temperature and pour point of petroleum products using anautomatic instrument.1.2 The measuring range of the apparatus is from -95 to 45C, however the precision statements were derived only
5、 from sampleswith no flow point temperatures from -77 to +2C and samples with pour point in the temperature range of -58 to +12C.1.3 Pour point results from this test method can be reported at 1 or 3C intervals.1.4 The values stated in SI units are to be regarded as standard. No other units of measu
6、rement are included in this standard.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 appropriate safety and health practices and determine the applicability of regulatorylimit
7、ations prior to use.2. Referenced Documents2.1 ASTM Standards:2D97 Test Method for Pour Point of Petroleum ProductsD4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD4177 Practice for Automatic Sampling of Petroleum and Petroleum ProductsD6300 Practice for Determination of Precis
8、ion and Bias Data for Use in Test Methods for Petroleum Products and LubricantsPractice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products and LubricantsD6708 Practice for Statistical Assessment and Improvement of Expected Agreement Between Two Test Methods t
9、hat Purportto Measure the Same Property of a Material3. Terminology3.1Definitions of Terms Specific to This Standard:3.1 Definitions:3.1.1 pour point, nin petroleum products, the lowest temperature at which movement of the test specimen is observed underthe prescribed conditions of the test.3.2 Defi
10、nitions of Terms Specific to This Standard:3.2.1 no-flow point, nin petroleum products, the temperature of the test specimen at which a wax crystal structure formationor viscosity increase, or both, is sufficient to impede movement of the surface of the test specimen under the conditions of the test
11、.3.1.1.13.2.1.1 DiscussionThe no-flow point occurs when, upon cooling, the formation of wax crystal structures or viscosity increase,1This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.07 onFlow P
12、roperties.Current edition approved July 15, 2007. Published August 2007. DOI: 10.1520/D7346-07.Current edition approved June 1, 2012. Published August 2012. Originally approved in 2007. Last previous edition approved in 2007 as D734607. DOI:10.1520/D734612.2For referenced ASTM standards, visit the A
13、STM 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 document is not an ASTM standard and is intended only to provide the user of an ASTM standard an
14、 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 appropriate. In all cases only the current versionof the standard as published by ASTM is to
15、 be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.or both, have progressed to the point where the applied observation device no longer detects movement under the conditions ofthe test.4. Summary of T
16、est Method4.1 After inserting the test specimen into the automatic no flow point apparatus and initiating the program, the test specimenis heated, if necessary, to a starting temperature and then cooled by prescribed rates. The test specimen is continuously tested forflow characteristics by continuo
17、usly monitoring the air pressure variation inside the test specimen vial. When the specimen is stillfluid, its movement will partially compensate for the reduction in air pressure in the test chamber above the test specimen surface.At some temperature the pressure measuring system detects a pressure
18、 decrease due to incapability of the test specimen to flowcaused by a crystal structure formation in the specimen or its viscosity increase, or both. This temperature is recorded as no flowpoint with a resolution of 0.1C. The pour point is recorded by rounding the no flow point temperature to either
19、 the next warmer1C interval or 3C interval. The test specimen is then reheated to allow for removal from the test chamber.5. Significance and Use5.1 The no flow point of a petroleum product is an index of the lowest temperature of its utility for some applications. Flowcharacteristics, such as no fl
20、ow point, can be critical for the proper operation of lubricating systems, fuel systems, and pipelineoperations.5.2 Petroleum blending operations require precise measurement of the no flow point.5.3 This test method can determine the temperature of the test specimen with a resolution of 0.1C at whic
21、h either crystals haveformed or viscosity has increased sufficiently, or both, to impede flow of the petroleum product.5.4 The pour point of a petroleum product is an index of the lowest temperature of its utility for certain applications. Flowcharacteristics, like pour point, can be critical for th
22、e correct operation of lubricating oil systems, fuel systems, and pipelineoperations.5.5 Petroleum blending operations require precise measurement of the pour point.5.6 Pour point results from this test method can be reported at either 1 or 3C intervals.5.7 This test method yields a pour point in a
23、format similar to Test Method D97/IP15 when the 3C interval results are reported.5.8 This test method has better repeatability and reproducibility relative to Test Method D97/IP15 as measured in the 2011interlaboratory test program (see 13.1.2).6. Apparatus (see Annex A1)6.1 Automatic No Flow Point
24、Apparatus3The apparatus consists of a microprocessorcontrolled test specimen chamber thatis capable of heating and cooling the test specimen at required rate, measuring the pressure inside the test specimen vial, andrecording the temperature of the test specimen chamber. A detailed description of th
25、e apparatus is provided in Annex A1.6.2 The apparatus shall be equipped with a thermostatically controlled specimen chamber, digital display, cooling and heatingsystems, pressure measuring system, and a specimen chamber temperature measuring device.6.3 The temperature measuring device in the specime
26、n chamber shall be capable of measuring the temperature from -105 to60C at a resolution of 0.1C.7. Reagents and Materials7.1 Specimen VialDisposable, clear glass cylinder with closed flat bottom, 1 mL capacity.Dimensions:Outer diameter: 8.0 to 8.3 mmWall thickness: 0.75 to 0.85 mmOuter length: 39.25
27、 to 40.25 mmNOTE 1Standard NWV type vial was found suitable for the application.7.2 Specimen Vial Stopper Disposable, proprietary designed for use in this apparatus.7.3 MicropipetteCapable of delivering 0.5 6 0.1 mL of sample. Positive displacement type micropipette with capillary pistonis preferred
28、 for use. Air-displacement type micropipettes are not recommended for viscous samples.8. Sampling8.1 Obtain a sample in accordance with Practice D4057 or D4177.8.2 At least 1 mL of sample is required for each test.8.3 Samples of very viscous materials can be warmed until they are reasonably fluid be
29、fore they are transferred; however, nosample shall be heated more than is absolutely necessary. The sample shall not be heated and transferred into the test specimencup unless its temperature is 70C or lower.3The sole source of supply of the apparatus known to the committee at this time is ISL model
30、 MPP 5Gs Analyzer, available from ISL, B.P. 70285 14653 Verson, France.If you are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meetingof the responsible technical committee, which you may att
31、end.D7346 122NOTE 2In the event the sample has been heated above this temperature, allow the sample to cool until its temperature is below 70C beforetransferring it.9. Preparation of Apparatus9.1 Prepare the apparatus for operation in accordance with the manufacturers instructions.10. Calibration an
32、d Standardization10.1 Ensure that all of the manufacturers instructions for calibration of the mechanical and electronic systems and operationof the apparatus are followed.10.2 To verify the performance of the apparatus, a sample for which extensive data has been obtained by no flow point testmethod
33、 may be used. Such verification materials can also be prepared from intra-company cross checks.11. Procedure11.1 Draw 0.5 6 0.1 mL of sample into a micropipette and transfer the specimen into a new clean, dry specimen vial. Whennecessary, heat the sample in a water bath or oven until it is just suff
34、iciently fluid to transfer. Samples with an expected no flowpoint above 25C or which appear solid at room temperature can be heated above 45C but shall not be heated above 70C (seeNote 2).NOTE 3Some samples like residual fuels, black oils, and cylinder stock have been known to be sensitive to therma
35、l history. In the case where suchsample is tested, refer to Test Method D97for sample treatment prior testing.11.2 Place a new clean, dry specimen vial stopper on the specimen vial and insert the assembly into the apparatus. Start theoperation of the apparatus according to the manufacturers instruct
36、ions. When the expected no flow point of the specimen is known,program it in the apparatus as EP (expected point) and start test sequence. From this point up to and including the termination ofthe test, recording and reporting of the result, the apparatus automatically controls the procedure.11.3 Th
37、e apparatus adjusts the specimen chamber to a preselected starting temperature. By default, the preselected startingtemperature is 25C. Alternatively, the operator can preprogram a defined starting temperature between 25 and 60C, if desired.When the expected no flow point is known and programmed in
38、the apparatus, the starting temperature shall be at least 30Cwarmer. In the event that the preselected starting temperature is programmed lower than 30C above the expected no flow point,the apparatus shall heat the specimen chamber to a starting temperature at least 30C above the expected no flow po
39、int, but notmore than 60C.11.4 When the expected no flow point of the specimen is not known, once the starting temperature is reached (see 11.3) thespecimen chamber is cooled at a rate of 1.5 6 0.15C/min.11.5 At the same time the cooling begins, the pressure measurement system is engaged to continuo
40、usly monitor specimenbehavior. When a decrease in pressure, as determined by the apparatus, is measured in the specimen vial, which signifies that thetest specimen has ceased to flow due to a crystal structure formation in the specimen or its viscosity increase, or both, thetemperature of the specim
41、en chamber is recorded as the no flow point and held on a digital display. The test chamber is thanreheated and the test sequence is terminated.11.6 When a no flow point is detected prematurely, as determined by the apparatus, the specimen is automatically reheated toa higher starting temperature, a
42、t least 30C warmer than the temperature of premature detection, and then cooled as described in11.4 until the no flow point is detected as described in 11.5.NOTE 4Some typical examples of premature no flow point are: when the NFP is detected during the fast cooling phase or when the NFP is detectedl
43、ess than 30C from the starting temperature.11.7 When the expected no flow point of the specimen is known, and programmed into the apparatus, once the startingtemperature (see 11.3) is reached, the specimen chamber is cooled at a rate of 10 6 1C/min until 30C warmer than theprogrammed expected no flo
44、w point, then the cooling rate is adjusted to 1.5 6 0.15C/min and the no flow point temperature isdetected as described in 11.5.11.8 When reporting of the pour point is desired, round the no flow point temperature in 11.5 to the next warmer 1C intervalor 3C interval, as specified, and record. Some a
45、pparatus are capable of performing this automatically.12. Report12.1 Report the temperature recorded in 11.5 with resolution of 0.1C, as the no-flow point in accordance with Test MethodD7346.12.2 Report the temperature recorded in 11.8 as the pour point at either the 1C interval or 3C interval as sp
46、ecified inaccordance with Test Method D7346.13. Precision and Bias13.1 PrecisionThe precision of this test method as determined by the statistical examination of the interlaboratory test resultsis as follows:D7346 12313.1.1 No Flow Point:413.1.1.1 RepeatabilityThe difference between two results obta
47、ined by the same operator with the same apparatus underconstant operating conditions on identical test material would, in the long run, in the normal and correct operation of this testmethod, exceed the following only in one case in twenty.1.93C Range: -77 to +2C13.1.213.1.1.2 ReproducibilityThe dif
48、ference between two single and independent results obtained by different operators workingin different laboratories on identical test material would, in the long run, in the normal and correct operation of this test method,exceed the following only in one case in twenty.2.62C Range: -77 to +2C13.1.2
49、 Pour Point at 3C Intervals:513.1.2.1 RepeatabilityThe difference between two results obtained by the same operator with the same apparatus underconstant operating conditions on identical test material would, in the long run, in the normal and correct operation of this testmethod, exceed the following only in one case in twenty.0.0384 50 X! range: 58 to 112 D7346-12_1 (1)X = result in C.13.1.2.2 ReproducibilityThe difference between two single and independent results obtained by different operators workingin differ
