ASTM D8049-2016 0967 Standard Test Method for Determining Concentration Count and Size Distribution of Solid Particles and Water in Light and Middle Distillate Fuels by Direct Imag.pdf

1、Designation: D8049 16Standard Test Method forDetermining Concentration, Count, and Size Distribution ofSolid Particles and Water in Light and Middle DistillateFuels by Direct Imaging Particle Analyzer1This standard is issued under the fixed designation D8049; the number immediately following the des

2、ignation indicates the year oforiginal adoption 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 uses a direc

3、t imaging particle analyzer(DIPA) to count and measure the size and shape of dispersedsolid particles and water droplets in light and middle distillatefuels in the overall range from 4 m to 100 m and in sizebands of 4 m, 6 m, and 14 m.NOTE 1Particle size data from 0.7 m through 300 m is available fo

4、ruse or reporting if deemed helpful.NOTE 2Shape is used to classify particles, droplets, and bubbles andis not a reporting requirement.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not purport to add

5、ress all of thesafety concerns, if any, associated 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:2D4057 Practic

6、e for Manual Sampling of Petroleum andPetroleum ProductsD4175 Terminology Relating to Petroleum Products, LiquidFuels, and LubricantsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD4306 Practice for Aviation Fuel Sample Containers forTests Affected by Trace Contamination2.2

7、ISO Standard:3ISO 12103-1 Road VehiclesTest Contaminants for FilterEvaluationPart 1: Arizona Test DustISO 11171 Hydraulic Fluid PowerCalibration of Auto-matic Particle Counters for Liquids2.3 MIL Standard:4MIL-PRF-5606 Hydraulic Fluid, Petroleum Base; Aircraft,Missile and Ordinance3. Terminology3.1

8、For definitions of terms used in this standard, refer toTerminology D4175.3.2 Definitions of Terms Specific to This Standard:3.2.1 air bubble, nnon-fuel, gaseous formations withinthe fuel, generally spherical in shape and visible as a heavywall ring due to the diffraction of light around and through

9、them.3.2.2 droplet, nnon-fuel liquid formations within the fuel,generally spherical in shape and visible as a thin wall ring dueto the diffraction of light around and through them.3.2.3 major particle diameter m, nthe maximum two-dimensional length of the particle measured3.2.4 minor particle diamet

10、er m, nthe maximum two-dimensional length of the particle measured perpendicular tothe major particle diameter.3.2.5 particle, nnon-liquid, non gaseous, solid objectsin the fuel.3.2.6 projected equivalent particle diameter m, nthediameter calculated from the projected area of a particle if thatarea

11、formed a circle, and in equation form is:Projected Equivalent Particle Diameter =area/0.785!1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.14 on Stability and Cleanliness of Liqu

12、id Fuels.Current edition approved June 1, 2016. Published July 2016. DOI: 10.1520/D8049-16.2For referenced ASTM standards, visit 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 Su

13、mmary page onthe ASTM website.3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.4For referenced MIL standards, visit the Defense Logistics Agency, DocumentServices website at http:/quicksearch.dla.milCopyright ASTM Internat

14、ional, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.3 Abbreviations:3.3.1 DIPADirect Imaging Particle Analyzer4. Summary of Test Method4.1 The optical measurement cell comprises a light sourceand an optical sensor. The principle of operation is theilluminatio

15、n and digital capture of actual particle images whichare then analyzed for size and shape by the system software.The visual capability of the instrument allows for the differ-entiation between solid, water, and air particles and thus thedetection of water and elimination of air bubbles from theanaly

16、sis.4.2 The test specimen, approximately 4 L, is agitated in itscontainer. The container is then fitted with a spigot to allowdelivery to the direct imaging particle analyzer (DIPA). Fluidflows through the DIPA and is analyzed for solids and watercontent. Larger or smaller volume test specimen may b

17、e usedas appropriate for the instrument.4.3 The method requires reporting of particle and dropletcounts in the 4m, 6 m, and 14 m categories, howeverparticle counts in the 0.7 m to 4 m size range may also bereported as well as additional ranges the user deems important.Particle size for this test met

18、hod shall be determined using thedefinition per 3.2.6.5. Significance and Use5.1 This test method is intended for use in the laboratory orin the field for evaluating the cleanliness of fuels identified inthe scope.5.2 Detection of particles and water can indicate degrada-tion of the fuel condition.

19、Particles, whether inorganic ororganic, can cause fouling of fuel filters and damage pumps,injectors, and pistons. Knowledge of particle size in relation tometallurgy can provide vital information, especially if thehardness of the solid particles are known from other sources.NOTE 3The method include

20、s the detection of water, solids, and airbubbles. The air bubbles are screened out of the data prior to analysis ofresults, based on shape and transparency, and are not reported in theresults.6. Apparatus56.1 Laboratory or Field Usage6.1.1 Direct Imaging Particle Analyzer (DIPA)Operatingon visual im

21、aging principles, comprising a flow cell withcamera/optics, light, test specimen container, and stand andsoftware to analyze the test specimen and display the particlemeasurement data.6.1.2 Test Specimen ContainerA clean fuel container forsample storage, transport, and transfer into the DIPA. Anepox

22、y-lined container of approximately 5 Lin volume has beenfound to be suitable, along with a nominal 19 mm or largeropening in the top lid for installation of a tube manifoldassembly to allow fuel transfer to the DIPA and air into theepoxy-lined container for venting.6.1.3 Tube Manifold AssemblyConsis

23、ts of a stopper orthreaded cap, which inserts into the top opening in the testspecimen container to seal it, and has through-holes whichaccept tubing for venting and tubing for flow of fuel to theDIPA.6.1.4 Flow ControllerThe flow of fuel through the DIPAis controlled by an orifice located in the ou

24、tflow line to thecollection container.6.1.5 Collection ContainerFor collecting analyzed fuelspecimen for possible retesting. Equivalent to the test specimencontainer.7. Reagents and Materials7.1 HeptaneReagent grade filtered through 0.45 m filter.7.2 Reticle, NIST, or other widely recognized standar

25、dsbody, traceable, for calibration of system. A 19 mm diameterreticle with 100 m grids and 10 m subdivisions has beenfound to work well for use in calibrating the instrument.7.3 Partistan Resolution Standard, mono disperse polymerbeads, coefficient of variation 10 %.7.4 Verification Standard Partist

26、an 2806, containing ISOMedium Test Dust, ISO 12103-A3 traceable to NIST.7.5 Partistan Super Clean Fluid.8. Sampling8.1 Sample into the test specimen container. Ensure it is newand unused, or in clean, new condition (see Practice D4306).Take precautions not to introduce contamination during thesampli

27、ng process.8.2 Take a representative sample. Refer to Practice D4057,Practice D4177, or other similar sampling practices.8.3 Confirm that the container is approximately 80 % filled(4 L).9. Preparation of Apparatus9.1 Ensure the DIPA is set up according to manufacturersinstructions.9.2 Ensure instrum

28、ent is clean and ready for use by flushingwith a filtered, fast drying solvent such as heptane. Cleansampling valve and tubing in the same manner. Systemcleanliness may be checked by running a sample of filteredheptane through it. If the test specimen has a 4 m count inexcess of 200 m mL the system

29、requires cleaning by contin-ued flushing with filtered heptane until the count falls below200.10. Test Specimen Preparation10.1 Gently shake the test specimen in its container for atleast 1 min to ensure that it is well mixed.10.1.1 To achieve a consistent agitation it is recommendedto either: (a) t

30、umble the test specimen container by hand orappropriate mechanical shaking device, (b) invert the containerback and forth for a minimum of 60 times at approximately1 Hz (cycle/second), or (c) use a roller device and roll for a5The sole source of supply of the apparatus known to the committee at this

31、 timeis Jet Fuel InFlow available from J.M. Canty Inc, 6100 Donner Rd., Lockport, NewYork USA 14094. If you are aware of alternative suppliers, please provide thisinformation to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical

32、 committee,1whichyou may attend.D8049 162minimum of 60 rotations. Other ways of gently shaking thecontainer may be used provided a well mixed test specimen isachieved.NOTE 4Over-shaken or mechanically stirred samples can result infinely dispersed micro bubbles that may be counted as solid particles.

33、Additionally, test specimens given ultrasonic treatment can result in thebreak up of agglomerated particles into smaller ones that can affect thecount.11. Apparatus Verification and Calibration11.1 Illumination level should be checked daily prior to useper manufacturers operating manual.11.2 Calibra

34、tion:11.2.1 The DIPA shall be calibrated per the manufacturersoperating manual. Calibration shall be done by referencing areticle (see 7.2). Once calibrated, a direct imaging typeinstrument remains in calibration as long as the camera andlens components remain unchanged and unmoved.11.2.2 The test s

35、pecimen flow rate should be similar forcalibration, verification, and operation. An orifice is providedon the outflow of the DIPA to ensure this.11.3 VerificationIt is recommended that verification beperformed at six month intervals.11.3.1 Particle CountUse the verification fluid referencedin 7.5 to

36、 verify particle count. Test in accordance with Section12. The per millilitre result obtained shall be equal to or lessthan r/1.414 of the measurement plus the uncertainty of theverification fluid from the certified 4 m(c) value of thestandard where r is the repeatability of the test (see Section 14

37、and Appendix X1). If the result obtained is not within thisfigure, ensure the sample preparation is in accordance with themanufacturers instructions, check the verification fluids valid-ity date and run a further test using the filtered heptane toconfirm the inlet tube and cell assembly are free fro

38、m contami-nants. Repeat the verification. If the result is still not within theallowed tolerance consult the operating manual or contact themanufacturer.NOTE 5Failure to correctly precondition the verification fluid canresult in particle counts not meeting the verification criteria specified bythe f

39、luid manufacturer.11.3.2 Particle SizeMono-disperse beads per 7.3,orsimilar, shall be used to verify the operation of the DIPA.Dilute the beads, if required, to an appropriate volume usingthe super clean fluid. The result of the analysis shall be within3 % of the average manufacturer certified parti

40、cle size plus thespecified standard deviation for the beads.12. Procedure12.1 Ensure the instrument is set up as indicated in themanufacturers instructions.12.2 Prepare the sample in the test specimen container perSection 10.12.3 Insert the stopper into the opening of the samplecontainer and attach

41、tubing.12.4 Ensure vent tube is within approximately 25 mm of thecontainer bottom and tubing for inflow is approximately25 mm inside the container.12.5 Invert the container and position approximately150 mm above the instrument ensuring tubing is straight andnot strained.12.6 The DIPA will fill and f

42、low will start. Allow the first500 mL to flow through to clean the DIPA. Start softwareanalysis at this point.12.7 The test specimen is run from the container through theDIPA and the resultant solid particle counts for the first 1000frames is compared to the results for a second 1000 frames inthe 1

43、m category. If the count values recorded in the 1mcategory are within either 10 % or 200 particles, then anaverage of the complete results of the first 1000 frames and thesecond 1000 frames is calculated and reported as the result.The solid particle count and water droplet count results will becalcu

44、lated based on the projected equivalent particle diameter.12.8 If solid particle count values recorded at 1 m are notwithin the specified error margin of 12.7, repeat the test.NOTE 6Volumes used in Section 12 may change according to therequired total volume the particular instrument requires for the

45、 analysis.13. Report13.1 Report the following:13.1.1 Reference this standard,13.1.2 Sample identification,13.1.3 Date of testing,13.1.4 Instrument model and software version,13.1.5 Solid particle cumulative counts per millilitre in the4 m, 6 m, and 14 m ranges. Additional ranges may bereported inclu

46、ding 0.7 m to 4 m,13.1.6 Water droplet cumulative counts per millilitre in the4 m, 6 m, and 14 m ranges. Additional ranges may bereported including 0.7 m to 4 m,NOTE 7Water droplets can stick to the inside of the container wallcausing reported water droplet count to be lower than actual.13.1.7 Solid

47、 particle size distribution (optional),13.1.8 Droplet size distribution (optional), and13.1.9 Any deviation from the method.NOTE 8With regard to 13.1.7 and 13.1.8 only, distributions can bereported based on count or volume, and by user preference of minordiameter, major diameter, equivalent particle

48、 diameter, area, perimeter, orany other characteristic measured. Distribution by any measure other thanequivalent particle diameter will be noted in the result report.14. Precision and Bias14.1 An interlaboratory study has yet to be completed. Atemporary statement including repeatability is reported

49、 inAppendix X1 which contains a description and results of thetesting done for this temporary precision statement. Fullprecision and bias statements based on interlaboratory roundrobin testing will be determined within five years of theadoption of this standard. The temporary repeatability to beused in 11.3.1 for particle count verification is r = 1088 (10 %)in the 4 m range when using verification fluid referenced in7.5.15. Keywords15.1 middle distillate fuels; particle analyzer; particle coun