Standard Test Method for Free Water and Particulate ...

1 Designation: D4176 04 (Reapproved 2009) Standard Test Method forFree Water and Particulate contamination in distillate Fuels(Visual Inspection Procedures)1 This Standard is issued under the fixed designation D4176; the number immediately following the designation 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 Standard has been approved for use by agencies of the Department of This test Method covers two procedures for estimatingthe presence of suspended free Water and solid particulatecontamination in distillate fuels having distillation end pointsbelow 400 C and an ASTM color of 5 or Both procedures can be used as field tests at storagetemperatures, or as laboratory tests at controlled Procedure 1 provides a rapid pass/fail Method forcontamination. Procedure 2 provides a gross numerical ratingof haze The values stated in SI units are to be regarded asstandard.

2 No other units of measurement are included in 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 Referenced standards :2D1500 Test Method for ASTM Color of Petroleum Products(ASTM Color Scale)D1744 Standard Test Method for Determination of Water inLiquid Petroleum Products by Karl Fischer Reagent3D2276 Test Method for Particulate Contaminant in AviationFuel by Line SamplingD2709 Test Method for Water and Sediment in MiddleDistillate Fuels by CentrifugeD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4860 Test Method for Free Water and Particulate Con-tamination in Middle distillate Fuels (Clear and BrightNumerical Rating) Adjuncts: distillate fuel Bar Chart4 distillate fuel Haze Rating Standard53. of Terms Specific to This (also termedclean-and-bright) acondition in which the fuel is free of haze or Water Water in excess of that soluble in the fuelat the temperature of the test, and appearing in the fuel as ahaze or cloudiness, or as small 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 instability, or protective-coating Summary of Test In Procedure 1 approximately 900 mL of fuel is placedinto a clear, glass, 1-L jar and is examined visually for sample is then swirled and examined for visual sedimentor Water drops below the In Procedure 2 approximately 900 mL of fuel is placedinto a clear, glass, 1-L jar and is examined visually for clarity is rated by placing a Standard bar chart behind thesample and comparing its visual appearance with the standardhaze rating photos.

3 The sample is then swirled and examinedfor visual sediment or Water drops below the When field testing, both Procedures 1 and 2 are per-formed immediately after sampling and at storage When lab testing, both Procedures 1 and 2 are per-formed after the sample has equilibrated at the test temperatureof test Method is under the jurisdiction of ASTM CommitteeD02onPetroleum Products and Lubricants and is the responsibility of Stability and Cleanliness of Liquid edition approved June 1, 2009. Published August 2009. Originallyapproved in 1982. Last previous edition approved in 2004 as D4176 04 1. referenced ASTM standards , visit the ASTM website, , orcontact ASTM Customer Service at ForAnnual Book of ASTMS tandardsvolume information, refer to the Standard s Document Summary page onthe ASTM The last approved version of this historical Standard is referencedon from ASTM International Headquarters. Order Adjunct Original adjunct produced in from ASTM International Headquarters.

4 Order Adjunct Original adjunct produced in ASTM International, 100 Barr Harbor Drive Box C-700 West Conshohocken, Pennsylvania 19428-2959, United States5. Significance and It has long been the practice to include in fuel specifi-cations a requirement that the fuel beclear and bright and freeof visible Particulate matter(seeNote 1). However, there hasbeen no Standard Method for making this determination so thatpractices have differed. This test Method provides standardprocedures for the Clean and brightis sometimes used in place ofclear meaning is Procedure 1 provides a rapid pass/fail Method 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 MethodsD1744,D2276,D2709, andD4860, permit quantitative determinationsof contaminants. No relationship has been established betweenProcedure 2 and various quantitative Limited laboratory evaluations of samples that havefailed thisclear and brighttest indicate that an experiencedtester can detect as little as 40 ppm of free Water in the When a fuel is tested at low temperatures at or below thecloud point temperature of the fuel , small amounts of solid waxparticles may be confused with a Water -induced haze If an attempt is made to use the test with fuels darkerthan a color rating of 5 in Test MethodD1500, the presence offree Water or Particulate could be obscured and missed by Container, clear-glass, capable of L of fuel and having a diameter of 100610 Card (Bar Chart)

5 ,4laminated in clear plastic,having five parallel lines of different widths and meeting thefollowing of Card Stock, white paper 120 mm by180 mm Color, Width, and Spacing, five black lines ofincreasing widths, commencing with a line mm wide, thesecond line mm wide, and each succeeding line mmwider to a maximum of The lines shall be numbered from 1 through 5, withthe thinnest line being No. 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 The differences between these haze levels are 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 Sensing Device (TSD), capable of monitor-ing the observed test temperature to within an accuracy C (61 F) for use in laboratory tests that require mea-surements to be made at a specific Bath, of suitable dimensionsand capable of controlling the sample container C (61 F) of the desired temperature for labora-tory tests that require measurements to be made at a Sampling shall be consistent with the procedures Draw the sample directly into the sample containerusing the following Be sure the sampling valve is free of loose solidcontaminants.

6 If rust or other loose encrustations are present,remove with a cloth; then flush the sampling valve prior totaking the actual Rinse a clean test container thoroughly with the fuelbeing sampled. (Warning Flammable. See ) Draw approximately 900 mL of fuel into the containeras rapidly as possible. Use a full flush rather than permittingthe fuel sample to trickle Sample Testing Both 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 Do not subsample or transfer the sample to a second-ary container. Perform the test with the sample drawn in theoriginal sample Replace the sample container s closure with an airtight closure through which a calibrated temperature sensingdevice is immersed in the sample. Allow the sample containerto equilibrate in a temperature-controlled bath, bringing it todesired test temperature within the allowed tolerance.

7 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). 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 recording the sample test 1 Check 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 clear and bright. Record if Particulate matter or waterwas or was not viewed at the bottom of the 2 Place the sample container into a welllighted area, avoiding light reflections on the front of thecontainer as much as possible. Place the bar chart directlybehind the container, with the lines toward the container andparallel with the container bottom.

8 The narrowest line shouldbe at the bottom of the Directly facing the container and bar chart, comparethe appearance of the bar chart through the sample with theD4176 04 (2009)2standard 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 disappearance oflines as well as a gradual lightening of all the lines. Record thenumber of the photograph closest in appearance as the rating ofthe 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 Also record any special observation, such as aparticularly heavy contamination with Water or solids or adarker than usual color which made ratings For field tests , the report shall provide an adequatedescription of the sample including the type of fuel , the sourceof the fuel (the sampling point), and the date, time, andapproximate temperature of the sample.

9 The report shall alsoindicate the approximate temperature at which the test was runand that a field test was For lab tests , the report shall include the test tem-perature at which the sample was analyzed. The report shallalso indicate that a lab test was 1 The results of the test shall be shown aspassif: (A) The sample has been found to beclear and brighton visual observance, and (B) If there is no Water or particu-lates observed at the bottom of the vortex. The results shall bereported asfailif (A) or (B) conditions are not met. The reasonfor any failure should also be In addition to thepass/failreporting requirements , the individual sample qualities may be reported asfollows:Clear and Bright Pass or FailFree Water Pass (absent) or Fail (present) particulates Pass (absent) or Fail (present) 2 The 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.

10 Any special or unusual observations, such as darkerthan usual fuel color, shall also be Precision and 1 It is not practical to specify the precisionof the procedure because the test is apass/failtest, not aquantitative 2 A rigorous precision statement cannotbe developed according to ASTM Research Report 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 The 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 only one case in The 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 The reproducibility values 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.