1、Designation: D4176 04 (Reapproved 2014)Standard Test Method forFree Water and Particulate Contamination in Distillate Fuels(Visual Inspection Procedures)1This standard is issued under the fixed designation D4176; the number immediately following the designation indicates the year oforiginal adoption
2、 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.This standard has been approved for use by agencies of the U.S. Department of Defense.1.
3、 Scope1.1 This test method covers two procedures for estimatingthe presence of suspended free water and solid particulatecontamination in distillate fuels having distillation end pointsbelow 400C and an ASTM color of 5 or less.1.1.1 Both procedures can be used as field tests at storagetemperatures,
4、or as laboratory tests at controlled temperatures.1.1.2 Procedure 1 provides a rapid pass/fail method forcontamination. Procedure 2 provides a gross numerical ratingof haze appearance.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thiss
5、tandard.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 and determine the applica-bility of regulatory limitations prior to use.2. Refe
6、renced Documents2.1 ASTM Standards:2D1500 Test Method for ASTM Color of Petroleum Products(ASTM Color Scale)D1744 Test Method for Determination of Water in LiquidPetroleum Products by Karl Fischer ReagentD2276 Test Method for Particulate Contaminant in AviationFuel by Line SamplingD2709 Test Method
7、for Water and Sediment in MiddleDistillate Fuels by CentrifugeD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4860 Test Method for Free Water and Particulate Contami-nation in Middle Distillate Fuels (Clear and Bright Nu-merical Rating)2.2 ASTM Adjuncts:Distillate Fuel Bar Char
8、t3Distillate Fuel Haze Rating Standard43. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 clear-and-bright (also termed clean-and-bright )acondition in which the fuel is free of haze or cloudiness.3.1.2 free waterwater in excess of that soluble in the fuelat the temperature of th
9、e test, and appearing in the fuel as ahaze or cloudiness, or as droplets.3.1.3 particulatessmall solid or semisolid particles, some-times referred to as silt or sediment, that may or may not besuspended in the fuel as a result of contamination by air-blowndusts, corrosion by-products, fuel instabili
10、ty, or protective-coating deterioration.4. Summary of Test Method4.1 In Procedure 1 approximately 900 mL of fuel is placedinto a clear, glass, 1-L jar and is examined visually for clarity.The sample is then swirled and examined for visual sedimentor water drops below the vortex.4.2 In Procedure 2 ap
11、proximately 900 mL of fuel is placedinto a clear, glass, 1-L jar and is examined visually for clarity.Fuel clarity is rated by placing a standard bar chart behind thesample and comparing its visual appearance with the standardhaze rating photos. The sample is then swirled and examinedfor visual sedi
12、ment or water drops below the vortex.4.3 When field testing, both Procedures 1 and 2 are per-formed immediately after sampling and at storage temperatureconditions.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricantsand is the responsib
13、ility ofSubcommittee D02.14 on Stability and Cleanliness of Liquid Fuels.Current edition approved Oct. 1, 2014. Published November 2014. Originallyapproved in 1982. Last previous edition approved in 2009 as D4176 04 (2009).DOI: 10.1520/D4176-04R14.2For referenced ASTM standards, visit the ASTM websi
14、te, 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.3Available from ASTM International Headquarters. Order Adjunct No.ADJD417601. Original adjunct produced in 1991.4
15、Available from ASTM International Headquarters. Order Adjunct No.ADJD417602. Original adjunct produced in 1991.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14.4 When lab testing, both Procedures 1 and 2 are per-formed after the samp
16、le has equilibrated at the test temperatureof interest.5. Significance and Use5.1 It has long been the practice to include in fuel specifi-cations a requirement that the fuel be clear and bright and freeof visible particulate matter (see Note 1). However, there hasbeen no standard method for making
17、this determination so thatpractices have differed. This test method provides standardprocedures for the test.NOTE 1Clean and bright is sometimes used in place of clear andbright. The meaning is identical.5.2 Procedure 1 provides a rapid pass/fail method forcontamination in a distillate fuel. Procedu
18、re 2 provides a grossnumerical rating of haze appearance, primarily as a communi-cation tool. Other test methods, including Test Methods D1744,D2276, D2709, and D4860, permit quantitative determinationsof contaminants. No relationship has been established betweenProcedure 2 and various quantitative
19、methods.5.3 Limited laboratory evaluations of samples that havefailed this clear and bright test indicate that an experiencedtester can detect as little as 40 ppm of free water in the fuel.6. Interferences6.1 When a fuel is tested at low temperatures at or below thecloud point temperature of the fue
20、l, small amounts of solid waxparticles may be confused with a water-induced haze orcloudiness.6.2 If an attempt is made to use the test with fuels darkerthan a color rating of 5 in Test Method D1500, the presence offree water or particulate could be obscured and missed by theviewer.7. Apparatus7.1 C
21、ylindrical Container, clear-glass, capable of holding1.0 6 0.1 L of fuel and having a diameter of 100 6 10 mm.7.2 Paper Card (Bar Chart),3laminated in clear plastic,having five parallel lines of different widths and meeting thefollowing description:7.2.1 Characteristics of Card Stock, white paper 12
22、0 mm by180 mm long.7.2.2 Line Color, Width, and Spacing, five black lines ofincreasing widths, commencing with a line 0.6 mm wide, thesecond line 1.6 mm wide, and each succeeding line 1.6 mmwider to a maximum of 6.4 mm.7.2.3 The lines shall be numbered from 1 through 5, withthe thinnest line being N
23、o. 1.7.3 A series of standard photographs4of the bar chartthrough samples of differing haze levels, numbered from 1through 6. Photograph No. 1 is the clearest, while No. 6represents the densest haze.7.4 The differences between these haze levels are arbitraryand are not intended to represent equivale
24、nt increases insuspended water content or particulates. It is essential,therefore, that only the proper approved photos be used.7.5 Temperature Sensing Device (TSD), capable of moni-toring the observed test temperature to within an accuracy of60.5C (61F) for use in laboratory tests that require mea-
25、surements to be made at a specific temperature.7.6 Temperature-Controlled Bath, of suitable dimensionsand capable of controlling the sample container temperaturewithin 60.5C (61F) of the desired temperature for labora-tory tests that require measurements to be made at a specifictemperature.8. Sampli
26、ng8.1 Sampling shall be consistent with the procedures ofPractice D4057.8.2 Draw the sample directly into the sample containerusing the following procedure:8.2.1 Be sure the sampling valve is free of loose solidcontaminants. If rust or other loose encrustations are present,remove with a cloth; then
27、flush the sampling valve prior totaking the actual sample.8.2.2 Rinse a clean test container thoroughly with the fuelbeing sampled. (WarningFlammable. See Annex A1.1.)8.2.3 Draw approximately 900 mL of fuel into the containeras rapidly as possible. Use a full flush rather than permittingthe fuel sam
28、ple to trickle out.9. Sample Preparation9.1 Field TestingBoth Procedures 1 and 2 are to beperformed immediately after drawing the sample. Record theapproximate sample storage temperature and the approximateambient temperature at which the test is performed.9.2 Laboratory Testing:9.2.1 Do not subsamp
29、le or transfer the sample to a second-ary container. Perform the test with the sample drawn in theoriginal sample container.9.2.2 Replace the sample containers closure with an airtight closure through which a calibrated temperature sensingdevice is immersed in the sample. Allow the sample containert
30、o equilibrate in a temperature-controlled bath, bringing it todesired test temperature within the allowed tolerance. Periodi-cally agitate the sample in a manner sufficient to homogenizethe bulk of the sample (water droplets and particulates, ifpresent, do not need to be evenly dispersed).9.2.3 Remo
31、ve the sample container from the temperature-controlled bath, wipe dry with an absorbent material (if a liquidbath is used), and perform the desired procedure(s) withminimal delay after removal. Remove the temperature sensingdevice after recording the sample test temperature.10. Procedure10.1 Proced
32、ure 1Check visually for evidence of water orparticulate contamination. Hold the sample up to the light andvisually examine for haze or lack of clarity. Swirl the sample toproduce a vortex and examine the bottom of the vortex forparticulate matter. Record the visual clarity as clear and brightor not
33、clear and bright. Record if particulate matter or waterwas or was not viewed at the bottom of the vortex.D4176 04 (2014)210.2 Procedure 2Place the sample container into a welllighted area, avoiding light reflections on the front of thecontainer as much as possible. Place the bar chart directlybehind
34、 the container, with the lines toward the container andparallel with the container bottom. The narrowest line shouldbe at the bottom of the chart.10.2.1 Directly facing the container and bar chart, comparethe appearance of the bar chart through the sample with thestandard photographs. Place the phot
35、ographs next to thecontainer so that they are lighted similarly to the sample. Selectthe photograph closest in appearance to the sample. Ignoredifferences in fuel color. Notice that the differences betweenphotographs consist both of the successive disappearance oflines as well as a gradual lightenin
36、g of all the lines. Record thenumber of the photograph closest in appearance as the rating ofthe sample.10.2.2 Remove the bar chart and swirl the sample containerto produce a vortex. Examine the bottom of the vortex forparticulate matter and water droplets. Record the presence ofany particulates or
37、water.10.2.3 Also record any special observation, such as aparticularly heavy contamination with water or solids or adarker than usual color which made ratings difficult.11. Report11.1 For field tests, the report shall provide an adequatedescription of the sample including the type of fuel, the sour
38、ceof the fuel (the sampling point), and the date, time, andapproximate temperature of the sample. The report shall alsoindicate the approximate temperature at which the test was runand that a field test was performed.11.1.1 For lab tests, the report shall include the test tem-perature at which the s
39、ample was analyzed. The report shallalso indicate that a lab test was performed.11.2 Procedure 1The results of the test shall be shown aspass if: (A) The sample has been found to be clear and brighton visual observance, and (B) If there is no water or particu-lates observed at the bottom of the vort
40、ex. The results shall bereported as fail if (A) or (B) conditions are not met. The reasonfor any failure should also be recorded.11.2.1 In addition to the pass/fail reporting requirements in11.2, the individual sample qualities may be reported asfollows:Clear and BrightPass or FailFree WaterPass (ab
41、sent) or Fail (present)ParticulatesPass (absent) or Fail (present)11.3 Procedure 2The report shall include the numericalrating of the sample and a note as to whether any particles orwater droplets were found on the bottom of the samplecontainer. Any special or unusual observations, such as darkertha
42、n usual fuel color, shall also be reported.12. Precision and Bias12.1 Procedure 1It is not practical to specify the precisionof the procedure because the test is a pass/fail test, not aquantitative measurement.12.2 Procedure 2Arigorous precision statement cannot bedeveloped according to ASTM Researc
43、h Report RR:D02-1007because the intervals between the rating steps are not known tobe equal. However, if the intervals are assumed to be equal, thefollowing estimates of precision will apply. Examination of theresults of a cooperative test program supports these estimates.12.2.1 RepeatabilityThe dif
44、ference between successiveresults obtained by the same operator with the same apparatusunder constant operating conditions on identical test sampleswould, in the long run, in the normal and correct operation ofthe test method, exceed one number in only one case in twenty.12.2.2 ReproducibilityThe di
45、fference between two singleand independent results obtained by different operators work-ing in different laboratories on identical test materials would, inthe long run, exceed two numbers only in one case out oftwenty.NOTE 2The reproducibility values above were estimated from resultsobtained at the
46、same location and on the same day by different operators/instruments testing identical samples at the same time as closely aspossible. The instability of typical fuel hazes introduces unpredictablevariations for samples tested at different times and makes the shipment ofsamples to different location
47、s impractical. The basis of this precisionstatement and the program comparing results obtained by this procedureby 12 operators on 24 fuel samples are available from ASTM Headquar-ters.12.3 No justifiable statement can be made on the bias ofeither procedure in Test Method D4176 because a fuel haze c
48、anresult from a number of causes and relationship with a singleabsolute quantitative method is not possible.13. Keywords13.1 cleanliness; distillate fuel; free water; particulate con-tamination; visual inspection; visual ratingsD4176 04 (2014)3ANNEX(Mandatory Information)A1. WARNING STATEMENTA1.1 Fl
49、ammable Liquid (General)A1.1.1 WarningFlammable.Keep away from heat, sparks, and open flame.Keep container closed.Use only with adequate ventilation.Avoid prolonged breathing of vapor or spray mist.Avoid prolonged or repeated contact with skin.Spillage and fire instructions will depend on nature of liquid.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 the validity of any such patent rights, an
