1、Designation: D5006 11An American National StandardStandard Test Method forMeasurement of Fuel System Icing Inhibitors (Ether Type) inAviation Fuels1This standard is issued under the fixed designation D5006; the number immediately following the designation indicates the year oforiginal adoption or, i
2、n 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 Department of Defense.1. Scope*1.1
3、This test method covers a technique for measuring theconcentration of Diethylene Glycol Monomethyl Ether (Di-EGME) in aviation fuels.Ameasured volume of fuel, extractedwith a fixed ratio of water, is tested with a suitable refracto-meter to determine the concentration of fuel system icinginhibitor (
4、FSII) in fuel. Precision estimates have been deter-mined for the DiEGME additive using specific extraction ratioswith a wide variety of fuel types. The extraction ratios are highenough that portable handheld refractometers can be used, butnot so high as to sacrifice accuracy or linearity, or both, i
5、n the0.01 to 0.25 vol % range of interest.1.2 DiEGME is fully described in Specification D4171 andin other specifications.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 WARNINGMercury has been designated by manyregulato
6、ry agencies as a hazardous material that can causecentral nervous system, kidney and liver damage. Mercury, orits vapor, may be hazardous to health and corrosive tomaterials. Caution should be taken when handling mercury andmercury containing products. See the applicable product Ma-terial Safety Dat
7、a Sheet (MSDS) for details and EPAswebsitehttp:/www.epa.gov/mercury/faq.htmfor addi-tional information. Users should be aware that selling mercuryand/or mercury containing products into your state or countrymay be prohibited by law.1.5 This standard does not purport to address all of thesafety conce
8、rns, 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:2D4171 Specification for Fuel System Icin
9、g InhibitorsE1 Specification for ASTM Liquid-in-Glass ThermometersE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE2251 Specification for Liquid-in-Glass ASTM Thermom-eters with Low-Hazard Precision Liquids3. Terminology3.1 Definitions of Terms Speci
10、fic to This Standard:3.1.1 analog refractometer, na traditional-style refracto-meter which visually projects a shadowline onto a scale etchedinto a glass reticle.3.1.1.1 DiscussionThe scale, which is magnified by aneyepiece, displays either a direct reading of DiEGME concen-tration, as is the case w
11、ith the analog HB refractometer, or maydisplay Brix units which must be converted into DiEGMEconcentration.3.1.2 Brix refractometer, na refractometer which displaysreadings on the Brix scale.3.1.3 Brix scale, nan expression of the mathematicalrelationship between refractive index and the concentrati
12、on byweight of pure sucrose in water.3.1.4 digital refractometer, nA refractometer which relieson a solid-state image sensor to measure the refractive index ofa solution, convert the refractive index reading into a particularunit of measure (percent DiEGME), and outputs the results ona digital displ
13、ay.3.2 Acronyms:1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.J0.04 on Additives and Electrical Properties.Current edition approved May 1, 2011. Published June 1, 2011. Originallyapproved in 1
14、989. Last previous edition approved in 2010 as D5006101. DOI:10.1520/D5006-11.2For 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 on
15、the ASTM website.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.2.1 DiEGMEDiethylene Glycol Monomethyl Ether3.2.2 FSIIfuel system icing inhibitor4. Summary of Test
16、Method4.1 In order to determine the concentration of DiEGME inaviation fuel, a measured volume of fuel is extracted with afixed ratio of water. The extraction procedure includes suffi-cient agitation and contacting time to ensure that equilibriumdistributions are attained. If using an Analog Refract
17、ometer,place several drops of water extract on the measuring surface,point it towards a light source, and take a reading on theinternal scale. The analog HB refractometer will display theactual percent volume of DiEGME on its scale. Users of a Brixrefractometer will follow a similar procedure, but w
18、ill have toconvert the Brix reading into DiEGME percent volume. If theBrix refractometer is not automatically temperature compen-sated, then a temperature correction must first be applied to theBrix reading before converting it to percent DiEGME. If usinga Digital Refractometer, place several drops
19、of water extract inthe sample well, press a button to initiate the reading, and thepercent volume of DiEGME will be displayed on the LCDdisplay. (WarningDiethylene glycol monomethyl ether (Di-EGME), slightly toxic material. This material caused slightembryo-fetal toxicity (delayed development) but n
20、o increase inbirth defects in laboratory animals. Consult the suppliersmaterial safety data sheets.)NOTE 1Isopropanol is not detected because of the similarity ofisopropanol/water refractive indices, and the presence of isopropanol infuel containing other additives results in lower than true values.
21、5. Significance and Use5.1 DiEGME is miscible with water and can be readilyextracted from the fuel by contact with water during shippingand in storage. Methods are therefore needed to check theadditive content in the fuel to ensure proper additive concen-tration in the aircraft.5.2 This test method
22、is applicable to analyses performed inthe field or in a laboratory.6. Apparatus6.1 RefractometerAn optical instrument used to measurethe physical properties of a solution. Refractometers suitablefor use in this test method include:6.1.1 HB Refractometer3An analog refractometer with adirect reading s
23、cale for percent DiEGME. This instrument isautomatically temperature compensated from 18 to 35C.6.1.2 Brix RefractometerAn analog refractometer with aBrix scale which may or may not be automatically temperaturecompensated.6.1.3 MISCO Jet Fuel Refractometer (p/n JPX-DiEGME)A digital refractometer tha
24、t provides a directreading of DiEGME concentration and is automatically tem-perature compensated within the range of 10 to 45C.6.1.4 Gammon HB2D RefractometerAdigital refractome-ter that provides a direct reading of DiEGME concentrationand is automatically temperature compensated within the rangeof
25、10 to 40C.6.2 Extraction VesselAny suitable vessel of at least 200mL with provisions for isolating a small column of waterextract at the bottom. Examples are separatory funnels, (glassor plastic), or plastic dropping bottles.6.3 Measuring VesselAny vessel capable of measuring upto 160 mL of fuel to
26、an accuracy of 6 2 mL, such as a 250-mLgraduated cylinder, or other calibrated container.6.4 Water Dispenser2.0-mL pipettes are preferred, butsyringes or burettes not exceeding 5.0-mL capacity that candispense 2.0 6 0.2 mL may be used. For the Brix refractome-ter, the pipette must measure 1.0 6 0.1
27、mL.6.5 ThermometerThe thermometer must have suitablerange to measure air and fuel temperature in the field.Accurateto 61C and meeting Specification E1 or any other tempera-ture measuring device that cover the temperature range ofinterest, such as thermocouples, thermistors, resistance tem-perature d
28、etectors (RTDs) or one conforming to SpecificationE2251 may be used that provides equivalent or better accuracyand precision than ASTM 1C.7. Reagents and Materials7.1 WaterDistilled or deionized water is preferred for theextraction procedure, and for refractometer calibration, butpotable water may b
29、e used.8. Refractometer Calibration8.1 All refractometers should be zero-set to water beforeuse. The exact procedure for zero-setting a refractometer variesbased on the type and make of instrument. Consult the usermanual for specific instructions on zero-setting each make ofrefractometer.8.2 The cal
30、ibration step is incorporated into the procedure tominimize the effect of temperature changes between the time ofcalibration and measurement. (WarningThe extraction, cali-bration, and measurement steps should be done at ambientconditions. Avoid placing the refractometer on hot or coldsurfaces, in po
31、ckets on your person, or other locations thatwould change the temperature of the instrument from ambient.When zero-setting or making a measurement, take care not toheat or cool the refractometer from ambient.)8.3 For the most accurate possible readings, the refractome-ter, the calibration fluid, and
32、 the ambient temperature should allbe in equilibrium within the temperature compensation range,or the operational temperature range, of the refractometer. Ifthere is a temperature disparity, allow some time for thetemperatures to equalize before taking a reading.9. Sample Preparation and Extraction9
33、.1 Extraction Ratios for Both Analog and Digital Refrac-tometers with Direct Reading DiEGME Scales:9.1.1 Measure 160 mLof fuel to be tested into the extractionvessel.3The analog HB refractometer and the digital HB2D refractometer are availablefrom Gammon Technical Products, Inc., 2300 Hwy 34, P.O. B
34、ox 400, Manasquan,NJ 08736. The MISCO Jet Fuel Refractometer (p/n JPX-DiEGME and Brixrefractometers are available from MISCO Refractometer, 3401 Virginia Rd.,Cleveland, Ohio 44122 USA. If you are aware of alternative suppliers, pleaseprovide this information to ASTM International Headquarters. Your
35、comments willreceive careful consideration at a meeting of the responsible technical committee,1which you may attend.D5006 1129.1.2 Measure 2.0 mL of water into the extraction vessel.9.2 Extraction Ratios for Analog Brix Refractometers Withor Without Automatic Temperature Compensation:9.2.1 Measure
36、80 mL of the fuel to be tested into theextraction vessel.9.2.2 Measure 1.0 mL of water into the extraction vessel.10. Sample Extraction10.1 Shake the extraction vessel vigorously for a minimumof 5 min for all fuels, preferably with the cap facing down.10.2 Mechanical shakers may be used, provided th
37、at thor-ough intermixing of the aqueous and fuel phases occurs,similar to that obtained by hand shaking. (WarningFollowing the extraction procedures is most critical. Failure toextract for the specified time or failure to provide vigorousagitation can result in false readings. If lower than expected
38、readings are obtained, a second test should be done with alonger extraction time.)10.3 Allow the extraction vessel to sit undisturbed at ambi-ent temperature for a period of at least 2 min to allow the waterto settle to the bottom.11. Sample Testing11.1 Measurement of Samples Using Digital Refractom
39、eterswith DiEGME Scales:11.1.1 Locate the thermometer and refractometer wherethey will remain at ambient temperature during the test.11.1.2 Isolate several drops of the water extract from theextraction vessel, and transfer to the sample well of the digitalrefractometer.11.1.3 If a separatory funnel
40、is used, it may be necessary tocollect some extract into a smaller container, and then transferseveral drops to the prism face with a clean eyedropper, syringeor pipette.11.1.4 If a dropping bottle is used as an extraction vessel,place it right side up, remove the cap, squeeze slightly, andreplace t
41、he cap with the bottle under a slight vacuum. Invert thebottle and allow the water extract to settle to the bottom. Uncapthe bottle and squeeze it gently until several drops of extractare collected on a tissue held in the same hand as therefractometer, and then allow several drops of the water extra
42、ctto fall into the refractometer well.11.1.5 If using the MISCO Jet Fuel Refractometer, close theevaporation cover to help prevent evaporation of the sampleduring testing.11.1.6 Allow some time for the temperature of the refrac-tometer, fluid, and ambient environment to equalize.11.1.7 Initiate the
43、reading by pressing the “GO” Button onthe MISCO Jet Fuel Refractometer or the “READ” Button onthe Gammon HB2D Refractometer.11.1.8 Record the ambient temperature reading displayed onthe thermometer to the nearest degree Celsius.11.1.9 Make certain that the temperature displayed on thethermometer is
44、within the temperature compensation range ofthe refractometer.11.1.10 Record the reading on the refractometer digitaldisplay to two significant figures in volume percent DiEGME.11.1.11 Take four more readings of the same sample, andaverage the results.11.1.12 Properly dispose of test fluids, wash ap
45、paratus withsoap and water, and dry all items. (WarningTreat therefractometer as an optical instrument and avoid damage to thelens and window elements. Store the refractometer in aprotective cover or case.)11.2 Measurement of Samples Using Analog HB or AnalogBrix Refractometers:11.2.1 Locate the the
46、rmometer and refractometer wherethey will remain at ambient temperature during the test.11.2.2 Isolate several drops of the water extract from theextraction vessel, and place on the prism face.11.2.3 If a separatory funnel is used, it may be necessary tocollect some extract into a smaller container,
47、 and then transferseveral drops to the prism face with a clean eyedropper,syringe, or pipette.11.2.4 If a dropping bottle is used as an extraction vessel,place it right side up, remove the cap, squeeze slightly, andreplace the cap with the bottle under a slight vacuum. Invert thebottle and allow the
48、 water extract to settle to the bottom. Uncapthe bottle and squeeze it gently until several drops of extractare collected on a tissue held in the same hand as therefractometer, and then allow several drops of the water extractto fall onto the prism face.11.2.5 Slowly lower the prism cover into place
49、, point therefractometer at a light source, and look into the eyepiece.(WarningFuel entrained in the water may cause an indistinctrefractometer reading. In most cases fuel residue on an analogrefractometer can be eliminated by slowly lowering the refrac-tometer cover. The surface tension of water should sweep fueloff the prism surface.)11.2.6 Take the reading at the point the shadowline inter-sects the scale.11.2.7 If using a HB refractometer, record the reading totwo significant figures in volume percent DiEGME.11.2.8 If using a Brix refractometer,
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