Standard Test Method for Measurement of Fuel System Icing Inhibitors (Ether Type) in Aviation Fuels

SIGNIFICANCE AND USE
5.1 DiEGME is miscible with water and can be readily extracted from the fuel by contact with water during shipping and in storage. Methods are therefore needed to check the additive content in the fuel to ensure proper additive concentration in the aircraft.  
5.2 This test method is applicable to analyses performed in the field or in a laboratory.
SCOPE
1.1 This test method covers a technique for measuring the concentration of Diethylene Glycol Monomethyl Ether (DiEGME) in aviation fuels. A measured volume of fuel, extracted with a fixed ratio of water, is tested with a suitable refractometer to determine the concentration of fuel system icing inhibitor (FSII) in fuel. Precision estimates have been determined for the DiEGME additive using specific extraction ratios with a wide variety of fuel types. The extraction ratios are high enough that portable handheld refractometers can be used, but not so high as to sacrifice accuracy or linearity, or both, in the 0.01 % to 0.25 % by volume range of interest.  
1.2 DiEGME is fully described in Specification D4171 and in other specifications.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 WARNING—Mercury has been designated by many regulatory agencies as a hazardous substance that can cause serious medical issues. Mercury, or its vapor, has been demonstrated to be hazardous to health and corrosive to materials. Use Caution when handling mercury and mercury-containing products. See the applicable product Safety Data Sheet (SDS) for additional information. The potential exists that selling mercury or mercury-containing products, or both, is prohibited by local or national law. Users must determine legality of sales in their location.  
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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ASTM D5006-11(2021) - Standard Test Method for Measurement of Fuel System Icing Inhibitors (Ether Type) in Aviation Fuels
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D5006 − 11 (Reapproved 2021)
Standard Test Method for
Measurement of Fuel System Icing Inhibitors (Ether Type) in
Aviation Fuels
This standard is issued under the fixed designation D5006; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript 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. Scope ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
1.1 This test method covers a technique for measuring the
mendations issued by the World Trade Organization Technical
concentration of Diethylene Glycol Monomethyl Ether (Di-
Barriers to Trade (TBT) Committee.
EGME)inaviationfuels.Ameasuredvolumeoffuel,extracted
with a fixed ratio of water, is tested with a suitable refracto-
2. Referenced Documents
meter to determine the concentration of fuel system icing
2.1 ASTM Standards:
inhibitor (FSII) in fuel. Precision estimates have been deter-
D4171 Specification for Fuel System Icing Inhibitors
minedfortheDiEGMEadditiveusingspecificextractionratios
E1 Specification for ASTM Liquid-in-Glass Thermometers
with a wide variety of fuel types.The extraction ratios are high
E29 Practice for Using Significant Digits in Test Data to
enough that portable handheld refractometers can be used, but
Determine Conformance with Specifications
not so high as to sacrifice accuracy or linearity, or both, in the
E2251 Specification for Liquid-in-Glass ASTM Thermom-
0.01 % to 0.25 % by volume range of interest.
eters with Low-Hazard Precision Liquids
1.2 DiEGME is fully described in Specification D4171 and
in other specifications.
3. Terminology
1.3 The values stated in SI units are to be regarded as
3.1 Definitions of Terms Specific to This Standard:
standard. No other units of measurement are included in this
3.1.1 analog refractometer, n—a traditional-style refracto-
standard.
meter which visually projects a shadowline onto a scale etched
1.4 WARNING—Mercury has been designated by many into a glass reticle.
regulatory agencies as a hazardous substance that can cause 3.1.1.1 Discussion—The scale, which is magnified by an
serious medical issues. Mercury, or its vapor, has been dem- eyepiece, displays either a direct reading of DiEGME
onstrated to be hazardous to health and corrosive to materials. concentration, as is the case with the analog HB refractometer,
Use Caution when handling mercury and mercury-containing or may display Brix units which must be converted into
products. See the applicable product Safety Data Sheet (SDS) DiEGME concentration.
for additional information. The potential exists that selling
3.1.2 Brix refractometer, n—a refractometer which displays
mercury or mercury-containing products, or both, is prohibited
readings on the Brix scale.
by local or national law. Users must determine legality of sales
3.1.3 Brix scale, n—an expression of the mathematical
in their location.
relationship between refractive index and the concentration by
1.5 This standard does not purport to address all of the
weight of pure sucrose in water.
safety concerns, if any, associated with its use. It is the
3.1.4 digital refractometer, n—A refractometer which relies
responsibility of the user of this standard to establish appro-
on a solid-state image sensor to measure the refractive index of
priate safety, health, and environmental practices and deter-
a solution, convert the refractive index reading into a particular
mine the applicability of regulatory limitations prior to use.
unit of measure (percent DiEGME), and outputs the results on
1.6 This international standard was developed in accor-
a digital display.
dance with internationally recognized principles on standard-
3.2 Acronyms:
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.J0.04 on Additives and Electrical Properties. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved May 1, 2021. Published June 2021. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1989. Last previous edition approved in 2016 as D5006 – 11 (2016). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D5006-11R21. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5006 − 11 (2021)
3.2.1 DiEGME—Diethylene Glycol Monomethyl Ether 6.1.3 MISCO Jet Fuel Refractometer (p/n JPX-
DiEGME)—A digital refractometer that provides a direct
3.2.2 FSII—fuel system icing inhibitor
reading of DiEGME concentration and is automatically tem-
perature compensated within the range of 10 °C to 45 °C.
4. Summary of Test Method
6.1.4 Gammon HB2D Refractometer—Adigital refractome-
4.1 In order to determine the concentration of DiEGME in
ter that provides a direct reading of DiEGME concentration
aviation fuel, a measured volume of fuel is extracted with a
andisautomaticallytemperaturecompensatedwithintherange
fixed ratio of water. The extraction procedure includes suffi-
of 10 °C to 40 °C.
cient agitation and contacting time to ensure that equilibrium
distributions are attained. If using an Analog Refractometer,
6.2 Extraction Vessel—Any suitable vessel of at least
place several drops of water extract on the measuring surface,
200 mL with provisions for isolating a small column of water
point it towards a light source, and take a reading on the extract at the bottom. Examples are separatory funnels, (glass
internal scale. The analog HB refractometer will display the
or plastic), or plastic dropping bottles.
actual percent volume of DiEGME on its scale. Users of a Brix
6.3 Measuring Vessel—Any vessel capable of measuring up
refractometer will follow a similar procedure, but will have to
to 160 mL of fuel to an accuracy of 62 mL, such as a 250 mL
convert the Brix reading into DiEGME percent volume. If the
graduated cylinder, or other calibrated container.
Brix refractometer is not automatically temperature
6.4 Water Dispenser—2.0 mL pipettes are preferred, but
compensated, then a temperature correction must first be
applied to the Brix reading before converting it to percent syringes or burettes not exceeding 5.0 mL capacity that can
dispense 2.0 mL 6 0.2 mL may be used. For the Brix
DiEGME. If using a Digital Refractometer, place several drops
ofwaterextractinthesamplewell,pressabuttontoinitiatethe refractometer, the pipette must measure 1.0 mL 6 0.1 mL.
reading, and the percent volume of DiEGME will be displayed
6.5 Thermometer—The thermometer must have suitable
on the LCD display. (Warning—Diethylene glycol monom-
range to measure air and fuel temperature in the field.Accurate
ethyl ether (DiEGME), slightly toxic material. This material
to 61 °C and meeting Specification E1 or any other tempera-
caused slight embryo-fetal toxicity (delayed development) but
ture measuring device that cover the temperature range of
no increase in birth defects in laboratory animals. Consult the
interest, such as thermocouples, thermistors, resistance tem-
suppliers’ material safety data sheets.)
perature detectors (RTDs) or one conforming to Specification
E2251 may be used that provides equivalent or better accuracy
NOTE 1—Isopropanol is not detected because of the similarity of
isopropanol/water refractive indices, and the presence of isopropanol in
and precision than ASTM 1C.
fuel containing other additives results in lower than true values.
7. Reagents and Materials
5. Significance and Use
7.1 Water—Distilled or deionized water is preferred for the
5.1 DiEGME is miscible with water and can be readily
extraction procedure, and for refractometer calibration, but
extracted from the fuel by contact with water during shipping
potable water may be used.
and in storage. Methods are therefore needed to check the
additive content in the fuel to ensure proper additive concen-
8. Refractometer Calibration
tration in the aircraft.
8.1 All refractometers should be zero-set to water before
5.2 This test method is applicable to analyses performed in
use.Theexactprocedureforzero-settingarefractometervaries
the field or in a laboratory.
based on the type and make of instrument. Consult the user
manual for specific instructions on zero-setting each make of
6. Apparatus
refractometer.
6.1 Refractometer—An optical instrument used to measure
the physical properties of a solution. Refractometers suitable 8.2 Thecalibrationstepisincorporatedintotheprocedureto
for use in this test method include: minimizetheeffectoftemperaturechangesbetweenthetimeof
6.1.1 HB Refractometer —An analog refractometer with a
calibration and measurement. (Warning—The extraction,
direct reading scale for percent DiEGME. This instrument is calibration, and measurement steps should be done at ambient
automatically temperature compensated from 18 °C to 35 °C.
conditions. Avoid placing the refractometer on hot or cold
6.1.2 Brix Refractometer—An analog refractometer with a surfaces, in pockets on your person, or other locations that
Brix scale which may or may not be automatically temperature
would change the temperature of the instrument from ambient.
compensated. When zero-setting or making a measurement, take care not to
heat or cool the refractometer from ambient.)
8.3 For the most accurate possible readings, the
The analog HB refractometer and the digital HB2D refractometer are available
refractometer, the calibration fluid, and the ambient tempera-
from Gammon Technical Products, Inc., 2300 Hwy 34, P.O. Box 400, Manasquan,
ture should all be in equilibrium within the temperature
NJ 08736. The MISCO Jet Fuel Refractometer (p/n JPX-DiEGME and Brix
refractometers are available from MISCO Refractometer, 3401 Virginia Rd.,
compensation range, or the operational temperature range, of
Cleveland, Ohio 44122 USA. If you are aware of alternative suppliers, please
the refractometer. If there is a temperature disparity, allow
provide this information toASTM International Headquarters. Your comments will
some time for the temperatures to equalize before taking a
receive careful consideration at a meeting of the responsible technical committee,
which you may attend. reading.
D5006 − 11 (2021)
9. Sample Preparation and Extraction 11.1.9 Make certain that the temperature displayed on the
thermometer is within the temperature compensation range of
9.1 Extraction Ratios for Both Analog and Digital Refrac-
the refractometer.
tometers with Direct Reading DiEGME Scales:
11.1.10 Record the reading on the refractometer digital
9.1.1 Measure160 mLoffueltobetestedintotheextraction
display to two significant figures in volume percent DiEGME.
vessel.
11.1.11 Take four more readings of the same sample, and
9.1.2 Measure 2.0 mL of water into the extraction vessel.
average the results.
9.2 Extraction Ratios for Analog Brix Refractometers With
11.1.12 Properly dispose of test fluids, wash apparatus with
or Without Automatic Temperature Compensation:
soap and water, and dry all items. (Warning—Treat the
9.2.1 Measure 80 mL of the fuel to be tested into the
refractometer as an optical instrument and avoid damage to the
extraction vessel.
lens and window elements. Store the refractometer in a
9.2.2 Measure 1.0 mL of water into the extraction vessel.
protective cover or case.)
10. Sample Extraction 11.2 Measurement of Samples Using Analog HB or Analog
Brix Refractometers:
10.1 Shake the extraction vessel vigorously for a minimum
11.2.1 Locate the thermometer and refractometer where
of 5 min for all fuels, preferably with the cap facing down.
they will remain at ambient temperature during the test.
10.2 Mechanical shakers may be used, provided that thor-
11.2.2 Isolate several drops of the water extract from the
ough intermixing of the aqueous and fuel phases occurs,
extraction vessel, and place on the prism face.
similar to that obtained by hand shaking. (Warning—
11.2.3 If a separatory funnel is used, it may be necessary to
Following the extraction procedures is most critical. Failure to
collect some extract into a smaller container, and then transfer
extract for the specified time or failure to provide vigorous
several drops to the prism face with a clean eyedropper,
agitation can result in false readings. If lower than expected
syringe, or pipette.
readings are obtained, a second test should be done with a
11.2.4 If a dropping bottle is used as an extraction vessel,
longer extraction time.)
place it right side up, remove the cap, squeeze slightly, and
10.3 Allow the extraction vessel to sit undisturbed at ambi-
replacethecapwiththebottleunderaslightvacuum.Invertthe
ent temperature for a period of at least 2 min to allow the water
bottleandallowthewaterextracttosettletothebottom.Uncap
to settle to the bottom.
the bottle and squeeze it gently until several drops of extract
are collected on a tissue held in the same hand as the
11. Sample Testing
refractometer, and then allow several drops of the water extract
11.1 Measurement of Samples Using Digital Refractometers to fall onto the prism face.
with DiEGME Scales:
11.2.5 Slowly lower the prism cover into place, point the
11.1.1 Locate the thermometer and refractometer where
refractometer at a light source, and look into the eyepiece.
they will remain at ambient temperature during the test.
(Warning—Fuelentrainedinthewatermaycauseanindistinct
11.1.2 Isolate several drops of the water extract from the
refractometer reading. In most cases fuel residue on an analog
extraction vessel, and transfer to the sample well of the digital
refractometer can be eliminated by slowly lowering the refrac-
refractometer.
tometer cover. The surface tension of water should sweep fuel
11.1.3 If a separatory funnel is used, it may be necessary to
off the prism surface.)
collect some extract into a smaller container, and then transfer
11.2.6 Take the reading at the point the shadowline inter-
severaldropstotheprismfacewithacleaneyedropper,syringe
sects the scale.
or pipette.
11.2.7 If using a HB refractometer, record the reading to
11.1.4 If a dropping bottle is used as an extraction vessel,
two significant figures in volume percent DiEGME.
place it right side up, remove the cap, squeeze slightly, and
11.2.
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