Designation: D381 – 12

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 Department of Defense.

1. Scope* 2. Referenced Documents

1.1 This test method covers the determination of the existent 2.1 ASTM Standards:2
gum content of aviation fuels, and the gum content of motor D1655 Specification for Aviation Turbine Fuels
gasolines or other volatile distillates in their finished form, D4057 Practice for Manual Sampling of Petroleum and
(including those containing alcohol and ether type oxygenates Petroleum Products
and deposit control additives—see Note 7 for additional E1 Specification for ASTM Liquid-in-Glass Thermometers
information) at the time of test. E29 Practice for Using Significant Digits in Test Data to
1.2 Provisions are made for the determination of the heptane Determine Conformance with Specifications
insoluble portion of the residue of non-aviation fuels. 2.2 Energy Institute Standard:3
1.3 The values stated in SI units are to be regarded as IP Standard Methods for Analysis and Testing of Petroleum
standard. No other units of measurement are included in this Products
standard. IP 540 Determination of the existent gum content of avia-
1.3.1 The accepted SI unit of pressure is the Pascal (Pa); the tion turbine fuel – jet evaporation method
accepted SI unit for temperature is degrees Celsius.
1.4 WARNING—Mercury has been designated by many 3. Terminology
regulatory agencies as a hazardous material that can cause 3.1 Definitions of Terms Specific to This Standard:
central nervous system, kidney and liver damage. Mercury, or 3.1.1 existent gum, n—the evaporation residue of aviation
its vapor, may be hazardous to health and corrosive to fuels, without any further treatment.
materials. Caution should be taken when handling mercury and 3.2 For non-aviation fuels, the following definitions apply.
mercury containing products. See the applicable product Ma- 3.3 solvent washed gum content, n—the residue remaining
terial Safety Data Sheet (MSDS) for details and EPA’s when the evaporation residue (see 3.4) has been washed with
website—http://www.epa.gov/mercury/faq.htm—for addi- heptane and the washings discarded.
tional information. Users should be aware that selling mercury 3.3.1 Discussion—For motor gasoline or non-aviation gaso-
and/or mercury containing products into your state or country line, solvent washed gum content was previously referred to as
may be prohibited by law. existent gum.
1.5 This standard does not purport to address all of the 3.4 unwashed gum content, n—the evaporation residue of
safety concerns, if any, associated with its use. It is the the product or component under test, without any further
responsibility of the user of this standard to establish appro- treatment.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For specific 4. Summary of Test Method
warning statements, see 6.4, 7.4, and 9.1. 4.1 When testing either aviation or motor gasoline, a 50 6
0.5 mL quantity of fuel is evaporated under controlled condi-
tions of temperature and flow of air (see Table 1). When testing
aviation turbine fuel, a 50 6 0.5 mL quantity of fuel is
evaporated under controlled conditions of temperature and

1 2
This test method is under the jurisdiction of ASTM Committee D02 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
D02.14 on Stability and Cleanliness of Liquid Fuels. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved April 15, 2012. Published May 2012. Originally the ASTM website.
3
approved in 1934. Last previous edition approved in 2009 as D381–09. DOI: Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,
10.1520/D0381-12. U.K.

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

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 D381 – 12
TABLE 1 Schedule of Test Conditions
Vaporizing Operating Temperature
Sample Type
Medium Bath Test Well
Aviation and motor gasoline air 160 to 165°C 150 to 160°C
Aviation turbine fuel steam 232 to 246°C 229 to 235°C

flow of steam (see Table 1). For aviation gasoline and aviation
turbine fuel, the resulting residue is weighed and reported as
milligrams per 100 mL. For motor gasoline, the residue is
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
Test Method D381 identified as the referee test method. Test Method D381 FIG. 1 Apparatus for Determining Gum Content by Jet
specifically requires the use of steam as the evaporating medium for Evaporation
aviation turbine fuels, whereas IP 540 allows either air or steam as the
evaporating medium for aviation turbine fuels.
conforming to Test Method D381 – 94, or earlier, are suitable.)
5. Significance and Use The bath should have wells and jets for two or more beakers.
5.1 The true significance of this test method for determining The rate of flow from each outlet when fitted with the conical
gum in motor gasoline is not firmly established. It has been adapters with 500 to 600 micron copper or stainless steel
proved that high gum can cause induction-system deposits and screens should not differ from 1000 mL/s by more than 15 %.
sticking of intake valves, and in most instances, it can be A liquid bath, if used, shall be filled to within 25 mm of the top
assumed that low gum will ensure absence of induction-system with a suitable liquid. Temperature shall be maintained by
difficulties. The user should, however, realize that the test means of thermostatic controls or by refluxing liquids of
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method is not of itself correlative to induction-system deposits. suitable composition.

The primary purpose of the test method, as applied to motor 6.5 Flow Indicator, as illustrated in Fig. 1, such as a
gasoline, is the measurement of the oxidation products formed flowmeter, capable of metering a flow of air or steam equiva-
in the sample prior to or during the comparatively mild lent to 1000 mL/s for each outlet.
conditions of the test procedure. Since many motor gasolines
NOTE 3—Alternatively, a pressure gage may be used to meter the flow
are purposely blended with nonvolatile oils or additives, the of air or steam equivalent to 1000 6 150 mL/s for each outlet.
heptane extraction step is necessary to remove these from the
evaporation residue so that the deleterious material, gum, may 6.6 Sintered Glass Filtering Funnel, coarse porosity,
be determined. With respect to aviation turbine fuels, large 150-mL capacity.
quantities of gum are indicative of contamination of fuel by 6.7 Steam—Supply by suitable means capable of delivering
higher boiling oils or particulate matter and generally reflect to the bath inlet the required amount of steam at 232 to 246°C.
poor handling practices in distribution downstream of the 6.8 Temperature Sensor, liquid-in-glass thermometer con-
refinery. forming to the requirements in the specification(s) for ASTM
3C/IP73C, found in Specification E1, or another temperature
6. Apparatus measuring device or system, or both, of at least equivalent
6.1 Balance, capable of weighing test specimens to the accuracy and precision over a temperature range from –5 to
nearest 0.1 mg. 400°C.
6.2 Beakers, of 100-mL capacity, as illustrated in Fig. 1. 6.9 Graduated Cylinders, with spout, capable of measuring
Arrange the beakers in sets, the number in each set depending 50 6 0.5 mL.
upon the number of beaker wells in the evaporating bath. Mark 6.10 Handling Equipment, forceps (stainless steel, spade
each beaker in the set, including the tare beaker, with an ended) or tongs (stainless steel) for use in handling the beakers
identifying number or letter. and conical jets, as required by this test method.
6.3 Cooling Vessel—A tightly covered vessel, such as a
7. Materials
desiccator without desiccant, for cooling the beakers before
weighing. 7.1 Air—Supply of filtered air at a pressure not more than
35 kPa.
NOTE 2—The use of a desiccant could lead to erroneous results. 7.2 Gum Solvent—A mixture of equal volumes of toluene
6.4 Evaporation Bath (Warning—If a liquid-filled evapo- and acetone.
ration bath is used, care must be taken that the flash point of the 7.3 Heptane—Minimum purity of 99.7 %.
liquid used is at least 30°C higher than the highest bath 7.4 Steam—Supply of steam free of oily residue and at a
temperature expected.) Either a solid metal block bath or a pressure not less than 35 kPa. (Warning—If a steam super-
liquid bath, electrically heated, and constructed in accordance heater is used, there may be exposed hot surfaces on the steam
with the general principles shown in Fig. 1 may be used. superheater. Avoid contact with exposed skin by use of
(Although all dimensions are given in SI units, older baths protective equipment as required.)

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 D381 – 12
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 6 90 mL/s for the outlet under test. Check the the total flow supplied to the outlets is at the appropriate rate,
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 6 90 mL/s from each outlet, at room
temperature and atmospheric pressure, will ensure delivery of 1000 6 150
10.2 Steam Flow:
mL/s at the temperature of 155 6 5°C for each outlet. It is recommended 10.2.1 Verify or calibrate the steam flow to ensure all outlets
to follow the manufacturers’ instructions to verify total flow/s (600 mL/s meet the 1000 6 150 mL/s steam flow requirement. Refer to
air flow 3 number of outlets = total flow/s) and uniformity from each the instrument manufacturer instructions for specific guidance
outlet. on performing the steam flow calibration procedure. Note the
8.2 Apply heat to the evaporation bath (see 6.4) until the setting of the flow indicator device for use with steam and use
temperature of the bath is between 160 and 165°C. Introduce this setting for subsequent tests.
air into the apparatus at a rate indicated on the flow indicator 10.2.1.1 One way to calibrate the steam flow, is to attach a
(see 6.5) from the exercise carried out in 8.1. Measure the copper tube to a steam outlet and extend the tube into a 2-L
temperature in each well with the temperature sensor (see 6.8) graduated cylinder that has been filled with crushed ice and
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placed with the bulb or sensor tip resting on the bottom of the water that has been previously weighed. Exhaust the steam into
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 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,
bath. When the temperature reaches 232°C, slowly introduce m = mass of graduated cylinder and ice, g,
k = mass of 1000 mL of steam at 232°C at atmospheric
dry steam into the system until a rate of 1000 6 150 mL/s for
pressure = 0.434 g, and
each outlet is reached (see 10.2). Regulate the temperature of
t = condensing time, s.
the bath to a range from 232 to 246°C to provide a well
temperature of 232 6 3°C. Measure the temperature with the
11. Procedure
temperature sensor, placed resting on the bottom of a beaker in
one of the bath wells with the conical adapter in place. Any 11.1 Wash the beakers, including the tare, with the gum
well having a temperature that differs by more than 3°C from solvent until free of gum. Rinse thoroughly with water and
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 6 90 mL/s air flow requirement as measured at with chromic acid cleaning solutions on used beakers (fresh
room temperature and atmospheric pressure. Refer to the chromic acid, 6-h soaking period, rinsing with distilled water
instrument manufacturer instructions for specific guidance on and drying). For this comparison visual appearance and mass
performing the air flow calibration procedure. Note the setting loss on heating the glassware under test conditions may be
of the flow indicator device for use with air and use this setting used. Detergent cleaning avoids the potential hazards and
for subsequent tests. inconveniences related to handling corrosive chromic acid
10.1.1.1 One way to calibrate the air flow is to use a solutions. The latter remains as the reference cleaning practice
calibrated flow indicator device, such as a flowmeter, separate and as such may function as an alternate to the preferred
from the device specified in 6.5, to check the air flow rate at procedure-cleaning with detergent solutions.
each outlet directly at room temperature and atmospheric 11.1.2 Remove the beakers from the cleaning solution by
pressure. To obtain accurate results, ensure that the back means of stainless steel forceps or tongs (see 6.10) and handle
pressure of the flowmeter is less than 1 kPa. only with forceps or tongs thereafter. Wash the beakers
10.1.1.2 Alternatively, another way to calibrate the air flow thoroughly, first with tap water and then with distilled water,
is to measure and adjust as appropriate the total air flow rate and dry in an oven at 150°C for at least 1 h. Cool the beakers
(mL/s) supplied to the outlets. The total air flow rate equals the for at least 2 h in the cooling vessel placed in the vicinity of the
expected air flow rate at each outlet times the number or outlet balance.

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 D381 – 12
11.2 Select the operating conditions, corresponding to the 11.8 For non-aviation fuels that have unwashed results that
aviation and motor gasoline or aircraft turbine fuel under test, are <0.5 mg/100 mL (see 11.6, Section 12, and 13.2) it is not
from the data given in Table 1. Heat the bath to the prescribed necessary to perform the washing steps identified in this
operating temperature. Introduce air or steam to the apparatus section, as well as in those that follow (11.9 to 11.12) since the
and adjust the total flow to that established in 8.1 or 9.2. If an washed gum value will always be # the unwashed gum value.
external preheater is used, regulate the temperature of the If the unwashed results are not <0.5 mg/100 mL, to each of the
vaporizing medium to give the prescribed test well tempera- beakers containing the residues from non-aviation fuels, add
ture. approximately 25 mL of heptane and swirl gently for 30 s.
11.3 Weigh the tare and test beakers to the nearest 0.1 mg. Allow the mixture to stand for 10 6 1 min. Treat the tare
Record the masses. 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
prevent the loss of any solid residue.
shake the contents of the sample container thoroughly using an
11.10 Repeat the extraction with a second portion of ap-
appropriate method. At atmospheric pressure, immediately
proximately 25 mL of heptane as described in 11.8 and 11.9. If,
filter a quantity of the sample through a sintered-glass funnel of
after the second extraction, the extract remains colored, repeat
coarse porosity (see 13.3). Treat the filtrate as described in
the extraction a third time. Do not perform more than three
11.5-11.7.
extractions (Note 6).
11.5 Measure a 50 6 0.5 mL test specimen in a graduated
cylinder (see 6.9), and transfer it to a weighed beaker (see 6.2). NOTE 6—Further extractions (after the third extraction) are not to be
performed, since portions of insoluble gum may be removed due to
(See Practice D4057 regarding sampling.) Use one beaker for
mechanical action, which could lead to lower solvent washed gum
each test specimen to be tested, and fill each beaker except the contents being determined.
tare. Place the filled beakers and the tare in the evaporation
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 to 165°C and, without replacing the
evaporation medium in an evaporation bath without a mechani- conical jets, allow the beakers to dry for 5 6 0.5 min.
cal means to raise and lower the conical jets, use forceps or 11.12 At the end of the drying period, remove the beakers
tongs (see 6.10) to replace the conical jet as each individual from the evaporation bath using forceps or tongs (see 6.10),
beaker is placed in the bath. When using steam, allow the place them in a cooling vessel, and allow them to cool in the
beakers to heat for 3 to 4 min before using forceps or tongs to vicinity of the balance for at least 2 h. Weigh the beakers in the
replace the conical jet (or lowering the conical jets by same manner as described in 11.3. Record the masses.
mechanical means), which shall be preheated either in the 12. Calculation
steam stream by placing on the steam outlet and positioning the
jet between the beaker wells or on top of the hot evaporation 12.1 Calculate the existent gum content of aviation fuels as
bath prior to attaching to the outlets. Using forceps or tongs (if follows:
needed), center each conical jet above the surface of the liquid, A 5 2000~B – D 1 X – Y! (2)
and start the flow of air or steam, adjusting it to the specified 12.2 Calculate the solvent washed gum content of motor
rate. Maintain the temperature and rate of flow, and allow the gasoline as follows:
test specimen to evaporate for 30 6 0.5 min.
S 5 2000~C – D 1 X – Z! (3)
NOTE 5—When introducing the flow of air or steam, care should be 12.3 Calculate the unwashed gum content of motor gasoline
taken to avoid splashing of the test specimen as this may lead to erroneous as follows:
low results.
U 5 2000~B – D 1 X– Y! (4)
11.6 At the end of the heating period, remove the conical
jets using forceps, tongs (see 6.10), or other suitable means, where:
and transfer the beakers from the bath to the cooling vessel. A = existent gum content, mg/100 mL,
Place the cooling vessel in the vicinity of the balance for at S = solvent washed gum content, mg/100 mL,
least 2 h. Weigh the beakers in accordance with 11.3. Record U = unwashed gum content, mg/100 mL,
the masses. B = mass recorded in 11.6 for the sample beaker plus
residue, g,
11.7 Segregate the beakers containing the residues from
C = mass recorded in 11.12 for the sample beaker plus
motor gasolines for finishing as described in 11.8 through
residue, g,
11.12. The remaining beakers may be returned for cleaning and D = mass recorded in 11.3 for the empty sample beaker, g,
reuse. X = mass recorded in 11.3 for the tare beaker, g,
11.7.1 Qualitative evidence of motor gasoline contamina- Y = mass recorded in 11.6 for the tare beaker, g, and
tion can be obtained by weighing the residue at this point if Z = mass recorded in 11.12 for the tare beaker, g.
retained samples of the original finished gasoline are available
for reference testing. This reference testing is essential since 13. Report
motor gasoline may contain deliberately added materials that 13.1 For aviation fuels with existent gum contents $1
are nonvolatile. If evidence of contamination is obtained, mg/100 mL, express the results to the nearest 1 mg/100 mL as
further investigation is indicated.
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existent gum content by Test Method D381. Round figures in

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 D381 – 12

FIG. 2 Precision for Existent Gum

accordance with Practice E29 or Appendix E of IP Standard material would, in the long run, in the normal and correct
Methods for Analysis and Testing of Petroleum and Related operation of the test method, exceed the values below only in
Products. For results <1 mg/100 mL, report as “<1 mg/100 one case in twenty.
mL.” r 5 1.11 1 0.095x for existent gum ~aviation gasoline!, (5)
13.2 For non-aviation fuels with either solvent washed or
unwashed gum content values $0.5 mg/100 mL, express the r 5 0.5882 1 0.2490x for existent gum
~aviation turbine fuel!, (6)
results to the nearest 0.5 mg/100 mL as either solvent washed
0.4
gum or unwashed gum content, or both, by Test Method D381. r 5 0.997x for unwashed gum content ~unwashed!, and (7)
Round figures in accordance with Practice E29 or Appendix E r 5 1.298x 0.3
for solvent washed gum content ~washed! (8)
of IP Standard Methods for Analysis and Testing of Petroleum
and Related Products. For results <0.5 mg/100 mL, report as where: x is the average of the results being compared.
“<0.5 mg/100 mL.” If the unwashed gum content is <0.5 14.1.2 Reproducibility—The difference between two test
mg/100 mL, the washed gum may also be reported as “<0.5 results independently obtained by different operators operating
mg/100 mL” (see 11.8). in different laboratories on nominally identical test material
13.3 For all fuels, if the filtration step (see 11.4) has been would, in the long run, in the normal and correct operation of
carried out before evaporation, the expression filtered shall the test method, exceed the values below only in one case in
follow the numerical value. twenty:
14. Precision and Bias 4 R 5 2.09 1 0.126x for existent gum ~aviation gasoline!, (9)

14.1 The precision, as obtained by statistical examination of R 5 2.941 1 0.2794x for existent gum
interlaboratory test results, is given in 14.1.1 and 14.1.2, and ~aviation turbine fuel!, (10)
illustrated graphically in Fig. 2. Analysis details are in the R 5 1.928xˆ 0.4 for unwashed gum content (11)
research report. R 5 2.494xˆ 0.3 for solvent washed gum content (12)
14.1.1 Repeatability—The difference between successive
test results, obtained by the same operator with the same where: x is the average of the results being compared.
apparatus under constant operating conditions on identical test NOTE 7—The precision values given above for solvent washed and
unwashed gum content were obtained on fourteen (14) finished motor
gasolines, which included two samples containing 10 volume % ethanol
4
Supporting data have been filed at ASTM International Headquarters and may and five (5) samples containing 15 volume % methyl tertiary butyl ether
be obtained by requesting Research Report RR:D02-1466. (MTBE), as well as deposit control additives as determined in a 1997
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 D381 – 12
interlaboratory study.4 The precision values for the solvent washed and 15. Keywords
unwashed gum content are based on samples containing between 0 to 15
mg/100 mL and 0 to 50 mg/100 mL gum content, respectively. 15.1 aviation fuels; existent gum; motor gasoline; solvent
14.2 Bias—Since there is no accepted reference material washed gum; unwashed gum
suitable for determining the bias for the procedure in Test
Method D381 for measuring existent gum (solvent washed or
unwashed gum), bias has not been determined.

SUMMARY OF CHANGES

Subcommittee D02.14 has identified the location of selected changes to this standard since the last issue
(D381–09) that may impact the use of this standard.

(1) Added mercury caveat to 1.4 in the Scope. (2) Updated terminology in Section 3.

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