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: D381 − 12 (Reapproved 2017)

Standard Test Method for

Gum Content in Fuels by Jet Evaporation1
This standard is issued under the fixed designation D381; 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 Development of International Standards, Guides and Recom-

1.1 This test method covers the determination of the existent mendations issued by the World Trade Organization Technical
gum content of aviation fuels, and the gum content of motor Barriers to Trade (TBT) Committee.
gasolines or other volatile distillates in their finished form, 2. Referenced Documents
(including those containing alcohol and ether type oxygenates
and deposit control additives—see Note 7 for additional 2.1 ASTM Standards:2
information) at the time of test. D1655 Specification for Aviation Turbine Fuels
D4057 Practice for Manual Sampling of Petroleum and
1.2 Provisions are made for the determination of the heptane Petroleum Products
insoluble portion of the residue of non-aviation fuels. E1 Specification for ASTM Liquid-in-Glass Thermometers
1.3 The values stated in SI units are to be regarded as E29 Practice for Using Significant Digits in Test Data to
standard. No other units of measurement are included in this Determine Conformance with Specifications
standard. 2.2 Energy Institute Standard:3
1.3.1 The accepted SI unit of pressure is the Pascal (Pa); the IP Standard Methods for Analysis and Testing of Petroleum
accepted SI unit for temperature is degrees Celsius. Products
1.4 WARNING—Mercury has been designated by many IP 540 Determination of the existent gum content of aviation
regulatory agencies as a hazardous material that can cause turbine fuel – jet evaporation method
central nervous system, kidney and liver damage. Mercury, or 3. Terminology
its vapor, may be hazardous to health and corrosive to
materials. Caution should be taken when handling mercury and 3.1 Definitions of Terms Specific to This Standard:
mercury containing products. See the applicable product Ma- 3.1.1 existent gum, n—the evaporation residue of aviation
terial Safety Data Sheet (MSDS) for details and EPA’s fuels, without any further treatment.
website—http://www.epa.gov/mercury/faq.htm—for addi- 3.2 For non-aviation fuels, the following definitions apply.
tional information. Users should be aware that selling mercury 3.3 solvent washed gum content, n—the residue remaining
and/or mercury containing products into your state or country when the evaporation residue (see 3.4) has been washed with
may be prohibited by law. heptane and the washings discarded.
1.5 This standard does not purport to address all of the 3.3.1 Discussion—For motor gasoline or non-aviation
safety concerns, if any, associated with its use. It is the gasoline, solvent washed gum content was previously referred
responsibility of the user of this standard to establish appro- to as existent gum.
priate safety and health practices and determine the applica- 3.4 unwashed gum content, n—the evaporation residue of
bility of regulatory limitations prior to use. For specific the product or component under test, without any further
warning statements, see 6.4, 7.4, and 9.1. treatment.
1.6 This international standard was developed in accor-
dance with internationally recognized principles on standard- 4. Summary of Test Method
ization established in the Decision on Principles for the 4.1 When testing either aviation or motor gasoline, a 50 mL
6 0.5 mL quantity of fuel is evaporated under controlled
1
This test method is under the jurisdiction of ASTM Committee D02 on
2
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Subcommittee D02.14 on on Stability, Cleanliness and Compatibility of Liquid contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Fuels. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved July 1, 2017. Published July 2017. Originally approved the ASTM website.
3
in 1934. Last previous edition approved in 2012 as D381 – 12. DOI: 10.1520/ Available from Energy Institute, 61 New Cavendish St., London, W1G 7AR,
D0381-12R17. U.K., http://www.energyinst.org.

*A Summary of Changes section appears at the end of this standard

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 D381 − 12 (2017)
TABLE 1 Schedule of Test Conditions
Vaporizing Operating Temperature
Sample Type
Medium Bath Test Well
Aviation and motor gasoline air 160 °C to 150 °C to
165 °C 160 °C

Aviation turbine fuel steam 232 °C to 229 °C to

246 °C 235 °C

conditions of temperature and flow of air (see Table 1). When

testing aviation turbine fuel, a 50 mL 6 0.5 mL quantity of fuel
is evaporated under controlled conditions of temperature and
flow of steam (see Table 1). For aviation gasoline and aviation
turbine fuel, the resulting residue is weighed and reported as FIG. 1 Apparatus for Determining Gum Content by Jet Evapora-
milligrams per 100 mL. For motor gasoline, the residue is tion
weighed before and after extracting with heptane and the
results reported as milligrams per 100 mL.
NOTE 1—Specification D1655 allows the existent gum of aviation
turbine fuels to be determined by either Test Method D381 or IP 540, with 6.4 Evaporation Bath (Warning—If a liquid-filled evapo-
Test Method D381 identified as the referee test method. Test Method D381 ration bath is used, care must be taken that the flash point of the
specifically requires the use of steam as the evaporating medium for liquid used is at least 30 °C higher than the highest bath
aviation turbine fuels, whereas IP 540 allows either air or steam as the
evaporating medium for aviation turbine fuels. temperature expected.) Either a solid metal block bath or a
liquid bath, electrically heated, and constructed in accordance
5. Significance and Use with the general principles shown in Fig. 1 may be used.
(Although all dimensions are given in SI units, older baths
5.1 The true significance of this test method for determining
conforming to Test Method D381 – 94, or earlier, are suitable.)
gum in motor gasoline is not firmly established. It has been The bath should have wells and jets for two or more beakers.
proved that high gum can cause induction-system deposits and The rate of flow from each outlet when fitted with the conical
sticking of intake valves, and in most instances, it can be adapters with 500 µm to 600 µm copper or stainless steel
assumed that low gum will ensure absence of induction-system screens should not differ from 1000 mL ⁄s by more than 15 %.
difficulties. The user should, however, realize that the test A liquid bath, if used, shall be filled to within 25 mm of the top
method is not of itself correlative to induction-system deposits. with a suitable liquid. Temperature shall be maintained by
The primary purpose of the test method, as applied to motor
means of thermostatic controls or by refluxing liquids of
gasoline, is the measurement of the oxidation products formed suitable composition.
in the sample prior to or during the comparatively mild
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conditions of the test procedure. Since many motor gasolines 6.5 Flow Indicator, as illustrated in Fig. 1, such as a
are purposely blended with nonvolatile oils or additives, the flowmeter, capable of metering a flow of air or steam equiva-
heptane extraction step is necessary to remove these from the lent to 1000 mL ⁄s for each outlet.
evaporation residue so that the deleterious material, gum, may NOTE 3—Alternatively, a pressure gage may be used to meter the flow
be determined. With respect to aviation turbine fuels, large of air or steam equivalent to 1000 mL ⁄s 6 150 mL ⁄s for each outlet.
quantities of gum are indicative of contamination of fuel by 6.6 Sintered Glass Filtering Funnel, coarse porosity,
higher boiling oils or particulate matter and generally reflect 150 mL capacity.
poor handling practices in distribution downstream of the
refinery. 6.7 Steam—Supply by suitable means capable of delivering
to the bath inlet the required amount of steam at 232 °C to
6. Apparatus 246 °C.
6.1 Balance, capable of weighing test specimens to the 6.8 Temperature Sensor, liquid-in-glass thermometer con-
nearest 0.1 mg. forming to the requirements in the specification(s) for ASTM
3C/IP73C, found in Specification E1, or another temperature
6.2 Beakers, of 100 mL capacity, as illustrated in Fig. 1.
measuring device or system, or both, of at least equivalent
Arrange the beakers in sets, the number in each set depending
accuracy and precision over a temperature range from –5 °C to
upon the number of beaker wells in the evaporating bath. Mark
400 °C.
each beaker in the set, including the tare beaker, with an
identifying number or letter. 6.9 Graduated Cylinders, with spout, capable of measuring
50 mL 6 0.5 mL.
6.3 Cooling Vessel—A tightly covered vessel, such as a
desiccator without desiccant, for cooling the beakers before 6.10 Handling Equipment, forceps (stainless steel, spade
weighing. ended) or tongs (stainless steel) for use in handling the beakers
NOTE 2—The use of a desiccant could lead to erroneous results. and conical jets, as required by this test method.

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 D381 − 12 (2017)
7. Materials on performing the air flow calibration procedure. Note the
7.1 Air—Supply of filtered air at a pressure not more than setting of the flow indicator device for use with air and use this
35 kPa. setting for subsequent tests.
10.1.1.1 One way to calibrate the air flow is to use a
7.2 Gum Solvent—A mixture of equal volumes of toluene calibrated flow indicator device, such as a flowmeter, separate
and acetone. from the device specified in 6.5, to check the air flow rate at
7.3 Heptane—Minimum purity of 99.7 %. each outlet directly at room temperature and atmospheric
7.4 Steam—Supply of steam free of oily residue and at a pressure. To obtain accurate results, ensure that the back
pressure not less than 35 kPa. (Warning—If a steam super- pressure of the flowmeter is less than 1 kPa.
heater is used, there may be exposed hot surfaces on the steam 10.1.1.2 Alternatively, another way to calibrate the air flow
superheater. Avoid contact with exposed skin by use of is to measure and adjust as appropriate the total air flow rate
protective equipment as required.) (mL/s) supplied to the outlets. The total air flow rate equals the
expected air flow rate at each outlet times the number or outlet
8. Assembly of Air-Jet Apparatus positions (for example, instrument has 5 positions and a total
8.1 Assemble the air-jet apparatus as shown in Fig. 1. With air flow rate measurement of 3000 mL ⁄s, indicating an ex-
the apparatus at room temperature, adjust the air flow to give a pected air flow rate of 600 mL ⁄s at each outlet). Once verifying
rate of 600 mL ⁄s 6 90 mL ⁄s for the outlet under test. Check the total flow supplied to the outlets is at the appropriate rate,
the remaining outlets for uniform air flow. perform uniformity checks by comparing the relative air flow
rates at each outlet position versus the requirements in 10.1.1.
NOTE 4—A rate of 600 mL ⁄s 6 90 mL ⁄s from each outlet, at room
temperature and atmospheric pressure, will ensure delivery of 1000 mL ⁄s 10.2 Steam Flow:
6 150 mL ⁄s at the temperature of 155 °C 6 5 °C for each outlet. It is 10.2.1 Verify or calibrate the steam flow to ensure all outlets
recommended to follow the manufacturers’ instructions to verify total meet the 1000 mL ⁄s 6 150 mL ⁄s steam flow requirement.
flow/s (600 mL ⁄s air flow × number of outlets = total flow/s) and Refer to the instrument manufacturer instructions for specific
uniformity from each outlet.
guidance on performing the steam flow calibration procedure.
8.2 Apply heat to the evaporation bath (see 6.4) until the Note the setting of the flow indicator device for use with steam
temperature of the bath is between 160 °C and 165 °C. and use this setting for subsequent tests.
Introduce air into the apparatus at a rate indicated on the flow 10.2.1.1 One way to calibrate the steam flow, is to attach a
indicator (see 6.5) from the exercise carried out in 8.1. Measure copper tube to a steam outlet and extend the tube into a 2 L
the temperature in each well with the temperature sensor (see graduated cylinder that has been filled with crushed ice and
6.8) placed with the bulb or sensor tip resting on the bottom of water that has been previously weighed. Exhaust the steam into
the beaker in the well. Do not use any well having a recorded the cylinder for approximately 60 s. Adjust the position of the
temperature outside the range from 150 °C to 160 °C. cylinder so that the end of the copper tube is immersed in the
water to a depth of less than 50 mm to prevent excessive back
9. Assembly of Steam-Jet Apparatus
pressure. After the appropriate time has elapsed, remove the
9.1 Assemble the steam-jet apparatus as shown in Fig. 1. copper tube from the cylinder and weigh the cylinder. The gain
(Warning—The sample and solvent vapors evaporated during in mass represents the amount of steam condensed. Calculate
the performance of this test procedure can be extremely the steam rate (mL/s) as follows:
flammable or combustible and hazardous from the inhalation
R 5 ~ M 2 m ! 1000/kt (1)
standpoint. The evaporation bath must be provided with an
effective exhaust hood to control such vapors and reduce the where:
risk of thermal explosion.) R = steam rate (mL/s),
9.2 To place the apparatus in operation, apply heat to the M = mass of graduated cylinder with condensed steam, g,

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bath. When the temperature reaches 232 °C, slowly introduce m = mass of graduated cylinder and ice, g,
dry steam into the system until a rate of 1000 mL ⁄s 6 k = mass of 1000 mL of steam at 232 °C at atmospheric
150 mL ⁄s for each outlet is reached (see 10.2). Regulate the pressure = 0.434 g, and
temperature of the bath to a range from 232 °C to 246 °C to t = condensing time, s.
provide a well temperature of 232 °C 6 3 °C. Measure the
temperature with the temperature sensor, placed resting on the 11. Procedure
bottom of a beaker in one of the bath wells with the conical 11.1 Wash the beakers, including the tare, with the gum
adapter in place. Any well having a temperature that differs by solvent until free of gum. Rinse thoroughly with water and
more than 3 °C from 232 °C is not suitable for standard tests. immerse in a mildly alkaline or neutral pH laboratory detergent
cleaning solution.
10. Calibration and Standardization 11.1.1 The type of detergent and conditions for its use need
10.1 Air Flow: to be established in each laboratory. The criterion for satisfac-
10.1.1 Verify or calibrate the air flow to ensure all outlets tory cleaning shall be a matching of the quality of that obtained
meet the 600 mL ⁄s 6 90 mL ⁄s air flow requirement as mea- with chromic acid cleaning solutions on used beakers (fresh
sured at room temperature and atmospheric pressure. Refer to chromic acid, 6 h soaking period, rinsing with distilled water
the instrument manufacturer instructions for specific guidance and drying). For this comparison visual appearance and mass

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 D381 − 12 (2017)
loss on heating the glassware under test conditions may be Place the cooling vessel in the vicinity of the balance for at
used. Detergent cleaning avoids the potential hazards and least 2 h. Weigh the beakers in accordance with 11.3. Record
inconveniences related to handling corrosive chromic acid the masses.
solutions. The latter remains as the reference cleaning practice 11.7 Segregate the beakers containing the residues from
and as such may function as an alternate to the preferred motor gasolines for finishing as described in 11.8 through
procedure-cleaning with detergent solutions. 11.12. The remaining beakers may be returned for cleaning and
11.1.2 Remove the beakers from the cleaning solution by reuse.
means of stainless steel forceps or tongs (see 6.10) and handle 11.7.1 Qualitative evidence of motor gasoline contamina-
only with forceps or tongs thereafter. Wash the beakers tion can be obtained by weighing the residue at this point if
thoroughly, first with tap water and then with distilled water, retained samples of the original finished gasoline are available
and dry in an oven at 150 °C for at least 1 h. Cool the beakers for reference testing. This reference testing is essential since
for at least 2 h in the cooling vessel placed in the vicinity of the motor gasoline may contain deliberately added materials that
balance. are nonvolatile. If evidence of contamination is obtained,
11.2 Select the operating conditions, corresponding to the further investigation is indicated.
aviation and motor gasoline or aircraft turbine fuel under test, 11.8 For non-aviation fuels that have unwashed results that
from the data given in Table 1. Heat the bath to the prescribed are <0.5 mg ⁄100 mL (see 11.6, Section 12, and 13.2) it is not
operating temperature. Introduce air or steam to the apparatus necessary to perform the washing steps identified in this
and adjust the total flow to that established in 8.1 or 9.2. If an section, as well as in those that follow (11.9 to 11.12) since the
external preheater is used, regulate the temperature of the washed gum value will always be less than or equal to the
vaporizing medium to give the prescribed test well tempera- unwashed gum value. If the unwashed results are not
ture. <0.5 mg ⁄100 mL, to each of the beakers containing the resi-

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dues from non-aviation fuels, add approximately 25 mL of
11.3 Weigh the tare and test beakers to the nearest 0.1 mg.
heptane and swirl gently for 30 s. Allow the mixture to stand
Record the masses.
for 10 min 6 1 min. Treat the tare beaker in the same manner.
11.4 If suspended or settled solid matter is present, mix or 11.9 Decant and discard the heptane solution, taking care to
shake the contents of the sample container thoroughly using an prevent the loss of any solid residue.
appropriate method. At atmospheric pressure, immediately
filter a quantity of the sample through a sintered-glass funnel of 11.10 Repeat the extraction with a second portion of ap-
coarse porosity (see 13.3). Treat the filtrate as described in 11.5 proximately 25 mL of heptane as described in 11.8 and 11.9. If,
– 11.7. after the second extraction, the extract remains colored, repeat
the extraction a third time. Do not perform more than three
11.5 Measure a 50 mL 6 0.5 mL test specimen in a gradu- extractions (Note 6).
ated cylinder (see 6.9), and transfer it to a weighed beaker (see
6.2). (See Practice D4057 regarding sampling.) Use one beaker NOTE 6—Further extractions (after the third extraction) are not to be
performed, since portions of insoluble gum may be removed due to
for each test specimen to be tested, and fill each beaker except mechanical action, which could lead to lower solvent washed gum
the tare. Place the filled beakers and the tare in the evaporation contents being determined.
bath, keeping the elapsed time between placing the first and 11.11 Place the beakers, including the tare, in the evapora-
last beaker in the bath to a minimum. When using air as the tion bath maintained at 160 °C to 165 °C and, without replac-
evaporation medium in an evaporation bath without a mechani- ing the conical jets, allow the beakers to dry for 5 min 6
cal means to raise and lower the conical jets, use forceps or 0.5 min.
tongs (see 6.10) to replace the conical jet as each individual
beaker is placed in the bath. When using steam, allow the 11.12 At the end of the drying period, remove the beakers
beakers to heat for 3 min to 4 min before using forceps or tongs from the evaporation bath using forceps or tongs (see 6.10),
to replace the conical jet (or lowering the conical jets by place them in a cooling vessel, and allow them to cool in the
mechanical means), which shall be preheated either in the vicinity of the balance for at least 2 h. Weigh the beakers in the
steam stream by placing on the steam outlet and positioning the same manner as described in 11.3. Record the masses.
jet between the beaker wells or on top of the hot evaporation
bath prior to attaching to the outlets. Using forceps or tongs (if 12. Calculation
needed), center each conical jet above the surface of the liquid, 12.1 Calculate the existent gum content of aviation fuels as
and start the flow of air or steam, adjusting it to the specified follows:
rate. Maintain the temperature and rate of flow, and allow the A 5 2000~ B 2 D1X 2 Y ! (2)
test specimen to evaporate for 30 min 6 0.5 min.
12.2 Calculate the solvent washed gum content of motor
NOTE 5—When introducing the flow of air or steam, care should be gasoline as follows:
taken to avoid splashing of the test specimen as this may lead to erroneous
low results. S 5 2000~ C 2 D1X 2 Z ! (3)

11.6 At the end of the heating period, remove the conical 12.3 Calculate the unwashed gum content of motor gasoline
jets using forceps, tongs (see 6.10), or other suitable means, as follows:
and transfer the beakers from the bath to the cooling vessel. U 5 2000~ B 2 D1X 2 Y ! (4)

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 D381 − 12 (2017)

FIG. 2 Precision for Existent Gum

where: <0.5 mg ⁄100 mL, the washed gum may also be reported as
A = existent gum content, mg/100 mL, “<0.5 mg ⁄100 mL” (see 11.8).
S = solvent washed gum content, mg/100 mL, 13.3 For all fuels, if the filtration step (see 11.4) has been
U = unwashed gum content, mg/100 mL, carried out before evaporation, the expression filtered shall
B = mass recorded in 11.6 for the sample beaker plus follow the numerical value.
residue, g,
C = mass recorded in 11.12 for the sample beaker plus 14. Precision and Bias4
residue, g,
D = mass recorded in 11.3 for the empty sample beaker, g, 14.1 The precision, as obtained by statistical examination of
X = mass recorded in 11.3 for the tare beaker, g, interlaboratory test results, is given in 14.1.1 and 14.1.2, and
Y = mass recorded in 11.6 for the tare beaker, g, and illustrated graphically in Fig. 2. Analysis details are in the
Z = mass recorded in 11.12 for the tare beaker, g. research report.
14.1.1 Repeatability—The difference between successive
13. Report test results, obtained by the same operator with the same
13.1 For aviation fuels with existent gum contents apparatus under constant operating conditions on identical test
≥1 mg ⁄100 mL, express the results to the nearest 1 mg ⁄100 mL material would, in the long run, in the normal and correct
as existent gum content by Test Method D381. Round figures operation of the test method, exceed the values below only in
in accordance with Practice E29 or Appendix E of IP Standard one case in twenty.
Methods for Analysis and Testing of Petroleum and Related r 5 1.1110.095x for existent gum ~ aviation gasoline! , (5)
Products. For results <1 mg ⁄100 mL, report as r 5 0.588210.2490x for existent gum (6)
“<1 mg ⁄100 mL.”
13.2 For non-aviation fuels with either solvent washed or ~ aviation turbine fuel! ,
unwashed gum content values ≥0.5 mg ⁄100 mL, express the r 5 0.997x 0.4 for unwashed gum content ~ unwashed! , and (7)
results to the nearest 0.5 mg ⁄100 mL as either solvent washed r 5 1.298x 0.3
for solvent washed gum content ~ washed! (8)
gum or unwashed gum content, or both, by Test Method D381.
Round figures in accordance with Practice E29 or Appendix E
of IP Standard Methods for Analysis and Testing of Petroleum 4
Supporting data have been filed at ASTM International Headquarters and may
and Related Products. For results <0.5 mg ⁄100 mL, report as be obtained by requesting Research Report RR:D02-1466. Contact ASTM Customer
“<0.5 mg ⁄100 mL.” If the unwashed gum content is Service at [email protected].

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 D381 − 12 (2017)
where: x is the average of the results being compared. NOTE 7—The precision values given above for solvent washed and
unwashed gum content were obtained on fourteen (14) finished motor
14.1.2 Reproducibility—The difference between two test gasolines, which included two samples containing 10 % by volume
results independently obtained by different operators operating ethanol and five (5) samples containing 15 % by volume methyl tertiary
in different laboratories on nominally identical test material butyl ether (MTBE), as well as deposit control additives as determined in
would, in the long run, in the normal and correct operation of a 1997 interlaboratory study.4 The precision values for the solvent washed
the test method, exceed the values below only in one case in and unwashed gum content are based on samples containing between
0 mg ⁄100 mL to 15 mg ⁄100 mL and 0 mg ⁄100 mL to 50 mg ⁄100 mL
twenty: gum content, respectively.
R 5 2.0910.126x for existent gum ~ aviation gasoline! , (9) 14.2 Bias—Since there is no accepted reference material
R 5 2.94110.2794x for existent gum (10) suitable for determining the bias for the procedure in Test
Method D381 for measuring existent gum (solvent washed or
~ aviation turbine fuel! , unwashed gum), bias has not been determined.
R 5 1.928x^0.4 for unwashed gum content (11)
15. Keywords
R 5 2.494x^0.3 for solvent washed gum content (12)
15.1 aviation fuels; existent gum; motor gasoline; solvent
where: x is the average of the results being compared. washed gum; unwashed gum

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