1、Designation: D7619 10Standard Test Method forSizing and Counting Particles in Light and Middle DistillateFuels, by Automatic Particle Counter1, 2This standard is issued under the fixed designation D7619; the number immediately following the designation indicates the year oforiginal adoption or, in t
2、he 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 specific automatic particlecounter2(APC) to count and measure
3、 the size of dispersed dirtparticles, water droplets and other particles, in light and middledistillate fuel, and bio fuels such as biodiesel and biodieselblends, in the overall range from 4 m(c) to 100 m(c) and inthe size bands $4 m(c), $6 m(c), and $14 m(c).NOTE 1ASTM specification fuels falling w
4、ithin the scope of this testmethod include Specifications: D975 grades 1D and 2D, D3699, D4814(see 14.1.1.1), D6751, D6985, D7467 and distillate grades of D396 andD2880.NOTE 2For the purposes of this test method, water droplets arecounted as particles, and agglomerated particles are detected and cou
5、ntedas a single larger particle. Dirt includes biological particles. Although theprojected area of a particle is measured, this is expressed as the diameterof a sphere for the purposes of this test method.NOTE 3The notation (c), used with particle sizes, is used to denotethat the apparatus has been
6、calibrated in accordance with ISO 11171.Strictly this only applies to particles up to 50 m.NOTE 4This test method may be used for particle sizes bands up to100 m(c), however the precision has only been determined for the sizebands $4 m(c), $6 m(c), and $14 m(c).1.2 The values stated in SI units are
7、to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not purport to address 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 a
8、nd determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:3D396 Specification for Fuel OilsD975 Specification for Diesel Fuel OilsD2880 Specification for Gas Turbine Fuel OilsD3699 Specification for KerosineD4057 Practice for Manual Sampling of
9、Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD4814 Specification for Automotive Spark-Ignition EngineFuelD5854 Practice for Mixing and Handling of Liquid Samplesof Petroleum and Petroleum ProductsD6300 Practice for Determination of Precision
10、and BiasData for Use in Test Methods for Petroleum Products andLubricantsD6751 Specification for Biodiesel Fuel Blend Stock (B100)for Middle Distillate FuelsD6985 Specification for Middle Distillate Fuel OilMilitary Marine Applications4D7467 Specification for Diesel Fuel Oil, Biodiesel Blend(B6 to B
11、20)2.2 ASTM Adjuncts:5ADJ6300 D2PP Determination of Precision and Bias datafor Use in Test Methods for Petroleum Products2.3 ISO Standards:61This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.14 on
12、Stability and Cleanliness of Liquid Fuels.Current edition approved May 1, 2010. Published August 2010.2The following equipment, as listed in RR:D02-1696, Seta-Avcount 91700-0available from Stanhope-Seta, London Street, Chertsey, Surrey KT16 8AP UK wasused to develop the precision statement. This lis
13、ting is not an endorsement orcertification by ASTM International.3For 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 Summary page onthe ASTM webs
14、ite.4Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.5For referenced ASTM adjuncts contact ASTM Customer Service atserviceastm.org.6Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.
15、org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.ISO 11171 Hydraulic Fluid PowerCalibration of Auto-matic Particle Counters for LiquidsISO 4406 Hydraulic Fluid PowerFluidsMethod forCoding Level of Contamination by Solid ParticlesI
16、SO 12103-A1 Specification for Ultra Fine Test Dust(UFTD)ISO 12103-A3 Specification for Medium Test Dust (MTD)3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 particles, nsolid particles and dispersed water drop-lets which are detected and counted by this test method.3.1.2 parti
17、cle count, nthe sum of the number of solidparticles and dispersed water droplets.3.1.3 particle size, m(c), nthe projected area equivalentdiameter of spherical particles passing through the detectingcell in accordance with ISO 11171.3.1.4 particle size cumulative count, nthe total number ofparticles
18、 per mL, in size bands,$4 m(c),$6 m(c), and$14m(c),3.1.4.1 DiscussionAutomatic particle counters may alsocount the total number of particles per mL, in size bands, inaddition to those in 3.1.4,upto$100 m.3.1.5 ISO Codes, na standard method for coding the levelof contamination by particles.3.1.5.1 Di
19、scussionResults are expressed by ISO Codes asspecified by ISO 4406. These codes are written in the form ofx/y/z, where x, y and z are ISO Codes equivalent to thecumulative counts, per mL, for particle size bands $4 m(c),$6 m(c), and $14 m(c) respectively. An example of this isgiven in Appendix X1.NO
20、TE 5All particle counts are per mL.3.1.6 coincidence error limit, nthe highest concentrationof ISO ultrafine test dust (ISO 12103-A1 or ISO UFTD) thatcan be counted with an automatic particle counter with lessthan 5 % error resulting from the presence of more than oneparticle in the sensor/laser opt
21、ical path at a time.3.1.7 test specimen, nan aliquot of the test sample. (SeeSection 10.)4. Summary of Test Method24.1 The optical measurement cell comprises a light sourceand an optical sensor. The principle of operation is themeasurement of laser light obscuration. Particles/droplets en-trained wi
22、thin the test specimen cast shadows on the opticalsensor causing a reduction of the output voltage of the sensor.The voltage drop is a function of the particle/droplet size. Eachdetected particle is counted, sized and recorded. Upon comple-tion of the test the software calculates and displays the nu
23、mberof obscuration events for each of the predetermined size bands.4.2 The test specimen is mixed in its container to suspendthe particles. Upon initiation of a test, the automatic particlecounter (APC) draws the test specimen directly from a testspecimen container (see Fig. A1.1). The test sequence
24、 com-mences by flushing the optical measurement cell and pipeworkwith 30 mL of the test specimen. This is immediately followedby the test of a 10 mL test specimen where particles in each ofthe specified size bands are counted. This flushing and mea-surement is then repeated. If the size band $4 m(c)
25、, per mL,measurements agree within either 10 % or 200 counts, themeasurements for each of the size bands are averaged for eachsize band to give results, per mL, for each size band.5. Significance and Use5.1 This test method is intended for use in the laboratory orin the field for evaluating the clea
26、nliness of distillate fuels, andliquid bio fuels. It is not applicable to on or in-line applications.5.2 This test method offers advantage over traditional filtra-tion methods in that it is a precise rapid test, and advantageover visual methods as it is not subjective.5.3 An increase in particle cou
27、nts can indicate a change inthe fuel condition caused by storage or transfer for example.5.4 High levels of particles can cause filter blockages andhave a serious impact on the life of pumps, injectors, pistonsand other moving parts. Knowledge of particle size in relationto the metallurgy can provid
28、e vital information especially if thehardness of particles is also known from other sources.5.5 This test method specifies a minimum requirement forreporting measurements in particle size bands (see A1.1.2).Some specific applications may require measurements in otherparticle size bands.5.6 Obtaining
29、 a representative sample and following therecommended sample and test specimen preparation proce-dures and timescales is particularly important with particlecounting methods. (See Sections 8, 10, 14.1.4 and Note 10.)6. Apparatus6.1 Automatic Particle Counter (APC)2Operating on thelaser light obscura
30、tion principle, comprising an optical mea-surement cell, bi-directional double pump, electronics andsoftware to analyze the test specimen, and display and print theparticle measurement data. (See Annex A1.)6.2 Test Specimen Container, cylindrical, made of glass orother suitable material, of at least
31、 125 mL volume withprovision for holding the test specimen input tube at least10 mm above the bottom of the container, and a cap with asuitable inert internal seal.NOTE 6It is recommended that glass test specimen containers shouldbe used to avoid any potential problems with particles adhering to the
32、insides of the containers due to static electricity that could occur withsome samples or some specimen containers.6.3 Waste Container, for collecting the tested test specimen.6.4 Filter Apparatus, general purpose for filtering heptaneor other solvents.6.4.1 Filters, cellulose, glass fiber or polycar
33、bonate0.45 m.6.5 Printer, to record details of the measurements andresults.D7619 1027. Reagents and Materials7.1 Verification and Calibration Fluids7Containing ISOMedium Test Dust (MTD) as specified in specificationISO 12103-A3.7.2 HeptaneReagent grade filtered down to 0.45 m.7.2.1 Prepare the hepta
34、ne by filtering through a 0.45 mfilter (see 6.4.1) contained in a filter apparatus (see 6.4) SeeNote 8. Store in a container prepared in accordance with 10.2.(WarningExtremely flammable, health hazard.)8. Sampling8.1 Unless otherwise specified, take a sample of at least 100mL in accordance with Prac
35、tices D4057, D5854, D4177,orother comparable sampling practices.8.2 It is essential to take a representative sample, but avoidpower mixing as this can modify the particles, break upagglomerated particles and entrain air. (See 14.1.4 and Note 7.)8.3 Use sample containers that are capable of transport
36、ingthe sample without contamination. Examples of these are fullyepoxy-lined metal or amber colored glass containers with athreaded cap, fitted with an inert liner, forming a seal with thecontainer.8.4 Prior to taking the sample, rinse the sample containerswith the product to be sampled at least thre
37、e times. Each rinseshall use product equal to 10 to 20 % of the container volume.A rinse shall include closing and shaking the container for aminimum of 5 s and then draining the product.8.5 Do not fill the sample container more than 90 % full.Overfilling affects the preparation of the test specimen
38、 asspecified in 10.1.8.6 Ensure that any aliquots or sub-division of the sampleresults in representative samples being taken and remaining inthe original sample container. Note 7 and 10.1 recommendsuitable procedures regarding this particle counting testmethod.9. Preparation of Apparatus9.1 Ensure t
39、hat the APC2is set up according to the instru-ment manufacturers operating instructions and the verificationand calibration requirements stated in both Section 11 andA1.1.4.9.2 Ensure that the mode of operation, specified for this testmethod by the manufacturer, is selected.9.3 Clean the outside of
40、the test specimen input tube beforeeach test sequence, by washing the outside in clean heptane oranother filtered solvent.9.4 At the start of any daily testing regime, initiate a testsequence using filtered heptane.9.5 If a test specimen is tested that has a $4 m(c)measurement of over 20 000 particl
41、es per mL, perform acomplete test sequence (two flushes and two measurements asshown in Section 12) using filtered heptane to clean and flushthe measurement cell and the inside of the connecting tubingbefore testing other test specimens.10. Test Specimen Preparation10.1 Gently shake the sample in it
42、s container, for at least aminute, sufficiently to ensure that a representative test speci-men can be drawn into the test specimen container.10.1.1 It is essential to take a representative test specimen,but avoid power mixing or vigorous mixing as this can modifythe particles, break up agglomerated
43、particles and entrain air.(See 14.1.4 and Note 17.)NOTE 7To achieve a consistent agitation, equivalent to “gentleshaking” of the sample, it is recommended to either: (a) tumble the samplecontainer, by hand or using a suitable automated mechanical tumbler, endover end for a minimum of 60 revolutions
44、at approximately 1 revolutionper second; (b) invert the sample container back and forth for a minimumof 60 times at approximately 1 cycle per second; or (c) use a barrel rollerand roll for a minimum of 60 rotations.Other ways of gently shaking the sample may be used, provided arepresentative test sp
45、ecimen is achieved.10.2 Use a clean test specimen container, or flush a testspecimen container by rinsing the inside of the container threetimes with the sample to be tested. Each rinse shall use productequal to 10 to 20 % of the container volume. A rinse shallinclude closing and shaking the contain
46、er for a minimum of 5s and then draining the product.Alternatively, the test specimencontainer may be cleaned by washing thoroughly with filteredheptane (see 7.2) and then allowed to dry in a clean environ-ment.NOTE 8The efficacy of cleaning of the test specimen container maybe checked by testing a
47、sample of filtered heptane (see 7.2), in the cleanedtest specimen container; this should give a count of less than 50 counts forthe $4 m(c) measurement.10.3 Immediately after gently shaking, pour the mixedsample into the test specimen container and fit a clean cap.Ensure that the test specimen conta
48、iner is less than 90 % full.NOTE 9Over shaken or mechanically stirred samples can result infinely dispersed micro bubbles forming that will be counted as solidparticles. Test specimens given ultrasonic treatment can result in thebreak-up of aglomerated particles into smaller ones that can affect the
49、particle counts.11. Apparatus2Verification and Calibration11.1 Verification:11.1.1 Verify the correct operation of the APC at least every6 months or more frequently if required by local qualitycontrols, by using the verification fluid (see 7.1) in accordancewith 11.1.1.1 and Section 12. The result obtained shall be equalto or less than R/=2 of the measurement plus the uncertaintyof the verification fluid, from the certified $4 m(c) value ofthe verification fluid, where R is the reproducibility of the test.If the result obtained is
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