1、Designation: D 4176 04e1An American National StandardStandard Test Method forFree Water and Particulate Contamination in Distillate Fuels(Visual Inspection Procedures)1This standard is issued under the fixed designation D 4176; the number immediately following the designation indicates the year ofor
2、iginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of
3、 Defense.e1NOTEThe word “not” was editorially added to paragraph 12.3 in March 2005.1. Scope*1.1 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
4、 of 5 or less.1.1.1 Both procedures can be used as field tests at storagetemperatures, 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 u
5、nits are to be regarded as thestandard. The values given in parentheses are for informationonly.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 p
6、ractices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1500 Test Method for ASTM Color of Petroleum Prod-ucts (ASTM Color Scale)D 1744 Test Method for Water in Liquid Petroleum Prod-ucts by Karl Fischer Reagent3D 2276 Test Method
7、 for Particulate Contaminant in Avia-tion Fuel by Line SamplingD 2709 Test Method for Water and Sediment in MiddleDistillate Fuels by CentrifugeD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4860 Test Method for Free Water and Particulate Con-tamination in Mid-Distillate Fue
8、ls (Clear and Bright Nu-merical Rating)2.2 ASTM Adjuncts:Distillate Fuel Bar Chart4Distillate Fuel Haze Rating Standard53. 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
9、.2 free waterwater in excess of that soluble in the fuelat the temperature of the 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
10、result of contamination by air-blowndusts, corrosion by-products, fuel instability, 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 e
11、xamined for visual sedimentor water drops below the vortex.4.2 In Procedure 2 approximately 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 st
12、andard1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the responsibility of SubcommitteeD02.14 on Stability and Cleanliness of Liquid Fuels.Current edition approved Nov. 1, 2004. Published November 2004. Originallyapproved in 1982. Last pr
13、evious edition approved in 2002 as D 4176 02.2For 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 Summary page onthe ASTM website.3Withdrawn.4Avai
14、lable from ASTM International Headquarters. Request Adjunct No.ADJD417601.5Available from ASTM International Headquarters. Request Adjunct No.ADJD417602.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohoc
15、ken, PA 19428-2959, United States.haze rating photos. The sample is then swirled and examinedfor visual sediment 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.4.4 When lab testing, both P
16、rocedures 1 and 2 are per-formed after the sample 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). Howeve
17、r, there hasbeen no standard method for making 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
18、 forcontamination in a distillate fuel. Procedure 2 provides a grossnumerical rating of haze appearance, primarily as a communi-cation tool. Other test methods, including Test MethodsD 1744, D 2276, D 2709, and D 4860, permit quantitativedeterminations of contaminants. No relationship has beenestabl
19、ished between Procedure 2 and various quantitativemethods.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
20、 at or below thecloud point temperature of the fuel, 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 D 1500, the presence offree water or particulate could be
21、 obscured and missed by theviewer.7. Apparatus7.1 Cylindrical 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),4laminated in clear plastic,having five parallel lines of different widths and meeting thefollowing description:
22、7.2.1 Characteristics of Card Stock, white paper 120 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 numbe
23、red from 1 through 5, withthe thinnest line being No. 1.7.3 A series of standard photographs5of 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
24、arbitraryand are not intended to represent equivalent increases insuspended water content or particulates. It is essential, there-fore, that only the proper approved photos be used.7.5 Temperature Sensing Device (TSD), capable of monitor-ing the observed test temperature to within an accuracy of60.5
25、C (61F) for use in laboratory tests that require mea-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 measu
26、rements to be made at a specifictemperature.8. Sampling8.1 Sampling shall be consistent with the procedures ofPractice D 4057.8.2 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 loos
27、e encrustations are present,remove with a cloth; then 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 possibl
28、e. Use a full flush rather than permittingthe fuel sample 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
29、 performed.9.2 Laboratory Testing:9.2.1 Do not subsample 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
30、is immersed in the sample. Allow the sample containerto 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, ifp
31、resent, do not need to be evenly dispersed).9.2.3 Remove 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 recordin
32、g the sample test temperature.10. Procedure10.1 Procedure 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
33、. Record the visual clarity as clear and brightD417604e12or not clear and bright. Record if particulate matter or waterwas or was not viewed at the bottom of the vortex.10.2 Procedure 2Place the sample container into a welllighted area, avoiding light reflections on the front of thecontainer as much
34、 as possible. Place the bar chart directlybehind 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 sam
35、ple with thestandard photographs. Place the photographs 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 disa
36、ppearance oflines as well as a gradual lightening 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 drop
37、lets. Record the presence ofany particulates or 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
38、 the sample including the type of fuel, the sourceof 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 sh
39、all include the test tem-perature at which the sample 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
40、particu-lates observed at the bottom of the vortex. 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 asfollow
41、s:Clear and BrightPass or FailFree WaterPass (absent) orFail (present)ParticulatesPass (absent) orFail (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 spec
42、ial or unusual observations, such as darkerthan 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 2A rigorous precision stateme
43、nt cannotbe developed according to ASTM Research Report RR: D02-1007 because the intervals between the rating steps are notknown to be equal. However, if the intervals are assumed to beequal, the following estimates of precision will apply. Exami-nation of the results of a cooperative test program s
44、upportsthese estimates.12.2.1 RepeatabilityThe difference 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 on
45、ly one case in twenty.12.2.2 ReproducibilityThe difference 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
46、 above were estimated from resultsobtained at the 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
47、makes the shipment ofsamples to different locations 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 pr
48、ocedure in Test Method D 4176 because a fuel hazecan result from a number of causes and relationship with asingle absolute quantitative method is not possible.13. Keywords13.1 cleanliness; distillate fuel; free water; particulate con-tamination; visual inspection; visual ratingsD417604e13ANNEX(Manda
49、tory Information)A1. WARNING STATEMENTA1.1 Flammable Liquid (General)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.SUMMARY OF CHANGESSubcommittee D02.14 has identified the location of selected changes to this standard since the last issue(D 4176 02) that may impact the use of this standard.(1) Updated 3.1.1 and 3.1.3. (2) Added 11
