ASTM D4870-09(2014)
(Test Method)Standard Test Method for Determination of Total Sediment in Residual Fuels
Standard Test Method for Determination of Total Sediment in Residual Fuels
SIGNIFICANCE AND USE
5.1 Appreciable amounts of sediment in a residual fuel oil can cause fouling of facilities for handling, and give problems in burner mechanisms. Sediment can accumulate in storage tanks, on filter screens, or on burner parts, resulting in obstruction of the flow of oil from the tank to the burner.
SCOPE
1.1 This test method covers the determination of total sediment up to 0.40 % m/m for distillate fuel oils containing residual components and to 0.50 % m/m in residual fuel oils having a maximum viscosity of 55 cSt (mm2/s) at 100°C. Some fuels can exceed the maximum filtration time specified in this test method due to factors other than the presence of significant quantities of insoluble organic or inorganic material. This test method can be used for the assessment of total sediment after regimes of fuel pretreatment designed to accelerate the aging process.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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 and health practices and determine the applicability of regulatory limitations prior to use. For specific warning statements, see 7.2, 7.3, Annex A1, and X1.6.1.
General Information
Relations
Buy Standard
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D4870 − 09 (Reapproved 2014)
Designation: 375/99
Standard Test Method for
Determination of Total Sediment in Residual Fuels
This standard is issued under the fixed designation D4870; 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.
1. Scope 3.1.1 total sediment—the sum of the insoluble organic and
inorganic material that is separated from the bulk of the
1.1 This test method covers the determination of total
residual fuel oil by filtration through a Whatman GF/A filter
sediment up to 0.40 % m/m for distillate fuel oils containing
medium, and that is also insoluble in a predominantly paraf-
residual components and to 0.50 % m/m in residual fuel oils
2 finic solvent.
havingamaximumviscosityof55cSt(mm /s)at100°C.Some
fuels can exceed the maximum filtration time specified in this
4. Summary of Test Method
testmethodduetofactorsotherthanthepresenceofsignificant
4.1 A weighed quantity (10 g) of the oil sample is filtered
quantities of insoluble organic or inorganic material. This test
through the prescribed apparatus at 100°C. After solvent
method can be used for the assessment of total sediment after
washing and drying the total sediment on the filter medium is
regimes of fuel pretreatment designed to accelerate the aging
weighed. The test is to be carried out in duplicate.
process.
1.2 The values stated in SI units are to be regarded as
5. Significance and Use
standard. No other units of measurement are included in this
5.1 Appreciable amounts of sediment in a residual fuel oil
standard.
can cause fouling of facilities for handling, and give problems
1.3 This standard does not purport to address all of the
in burner mechanisms. Sediment can accumulate in storage
safety concerns, if any, associated with its use. It is the
tanks, on filter screens, or on burner parts, resulting in
responsibility of the user of this standard to establish appro-
obstruction of the flow of oil from the tank to the burner.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For specific
6. Apparatus
warning statements, see 7.2, 7.3, Annex A1, and X1.6.1.
6.1 Filtration Apparatus, constructed of brass, with copper
steam coils attached, suitably supported above a vacuum flask
2. Referenced Documents
2 appropriately protected against the effects of implosion. See
2.1 ASTM Standards:
Figs. 1 and 2.
D4057 Practice for Manual Sampling of Petroleum and
Petroleum Products 6.2 Temperature Measuring Device , capable of measuring
thetemperatureintherangefrom95to105°Cwithanaccuracy
D4177 Practice for Automatic Sampling of Petroleum and
of 0.5°C.
Petroleum Products
E1 Specification for ASTM Liquid-in-Glass Thermometers
6.3 Oven, electric, capable of maintaining a temperature of
110 6 1°C. The oven should be capable of safely evaporating
3. Terminology
the solvent without risk of fire.
3.1 Definitions of Terms Specific to This Standard:
6.4 Stirring Rod, glass or polytetrafluoroethylene (PTFE)
approximately 150 mm in length and 3 mm in diameter.
6.5 Beaker, glass, 30 mLcapacity, either squat form with lip
This test method is under the jurisdiction of ASTM Committee D02 on
or conical.
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.14 on Stability and Cleanliness of Liquid Fuels.
6.6 Small Dishes, such as watch glasses or Petri dishes.
Current edition approved Dec. 1, 2014. Published February 2015. Originally
approved in 1988. Last previous edition approved in 2009 as D4870 – 09. DOI:
6.7 Hotplate, electric.
10.1520/D4870-09R14.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 6.8 Steam Generator, to provide steam at 100 6 1°C.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
6.9 Vacuum Source, capable of providing the specified
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. vacuum.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4870 − 09 (2014)
FIG. 1 Detail of Filtration Cell
6.15 Syringe or Graduated Wash Bottle , minimum capacity
25 mL, graduated in 0.5 mL increments.
6.16 Forceps, spade-ended.
7. Reagents and Materials
7.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
where such specifications are available. Other grades may be
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
FIG. 2 Arrangement of Filtration Apparatus
accuracy of the determination.
7.2 Normal Heptane, minimum 99.75 % purity.
(Warning—Flammable, vapor harmful if inhaled. See A1.1.)
6.10 Vacuum Gauge, capable of measuring the specified
7.3 Toluene, at least reagent grade purity. (Warning—
vacuum.
Flammable, vapor harmful. See A1.2.)
6.11 Filter Medium, Whatman glass fiber filter medium,
7.4 Wash Solvent, consisting of 85 volume % n-heptane
Grade GF/A, 47 mm diameter.
(7.2) and 15 volume % toluene (see 7.3).
6.12 High Speed Mixer, any convenient type, minimum
speed 400 rpm.
Reagent Chemicals, American Chemical Society Specifications, American
6.13 Desiccator.
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
listed by the American Chemical Society, see Annual Standards for Laboratory
6.14 Cooling Vessel, a desiccator or other type of tightly
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
covered vessel for cooling the filter media before weighing.
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
The use of a drying agent is not recommended. MD.
D4870 − 09 (2014)
NOTE4—Forsamplesofhighviscosityorhighsediment,levelfiltration
8. Sampling
will be aided by small stage or even dropwise addition. It is preferable to
8.1 Sample in accordance with Practice D4057 or Practice
avoid complete coverage of the filter medium with unfiltered oil sample.
D4177.
For samples of low filtration rate the pressure of 40 6 2 kPa should be
maintained for the 25-min period.
9. Procedure
9.5 Filter Washing—When the filtration is complete and the
upper filter medium appears dry, continue the steam and
9.1 Sample Preparation—Mix the whole sample, as
vacuum for a further 5 min. Discontinue the steam supply and
received, thoroughly using a high speed mixer when
cooltheapparatusbypassingtapwaterthroughthecoils.Wash
practicable, for 30 s. In all cases a sample taken on a glass or
the filtration unit carefully with two portions of 25 61mLof
PTFE rod dipped to the bottom of the container must show a
the wash solvent from a syringe or graduated wash bottle with
homogeneous appearance. For fuels with a high wax content
a fine nozzle, taking care to remove any adhered sample from
(high pour point), or of very high viscosity, the sample must be
the wall of the upper part of the apparatus. Carefully remove
heated before stirring. The temperature must be either 15°C
the top portion of the filtration unit and wash the rim of the
above the pour point in the case of low viscosity fuels, or that
filter with a further 10 6 0.5 mL of the wash solvent in a
equivalent to 150 to 250 cSt in the case of high viscosity fuels.
similar manner. Finally wash the whole of the filter medium
In no case should the temperature exceed 80°C.
area with 10 6 0.5 mL of n-heptane.
9.2 Filter Preparation—For each test, dry two filter media
NOTE 5—If the sample filters very rapidly, the vacuum should be
for 20 min in the oven at 110°C. Transfer each filter medium,
released before the first solvent washing, to ensure complete coverage of
separately, rapidly to a cooling vessel and allow to cool to
the filter medium area by solvent. The vacuum should then be gently
room temperature for 20 min. Weigh each filter medium to the
reapplied for the subsequent operations.
nearest 0.0001 g.
9.6 Apparatus Disassembly—After the filter medium ap-
NOTE 1—The Whatman GF/A filter media are fragile and are to be
pears dry, discontinue the vacuum supply. Using the forceps,
handled with care. Before use, check each medium for consistency, and
carefully remove each filter medium separately and transfer
the possible presence of small defects (holes).
them to the oven at 110°C. Dry for 20 min and quickly transfer
NOTE 2—For convenience, place the filters on numbered small dishes
(6.6) during drying and cooling. them to the cooling vessel (6.14). Allow them to cool to room
temperature for 20 min and reweigh them to the nearest 0.0001
9.3 Apparatus Assembly—Before use, check that the filter
g.
support screen is clean. If necessary, the screen must be
cleaned by boiling in a high boiling point aromatic solvent.
10. Calculation
When more than 2 % of the sinter area remains blocked by
10.1 Calculate the mass percentage of total sediment for
particulate matter after such cleaning, discard the screen and
each test specimen using Eq 1. For each test specimen with a
install a new one.
calculated total sediment concentration >0.005 % m/m as
9.3.1 The filtration unit must be clean and dry before
determined by Eq 1, record the mass percentage of total
assembly. Stack the two previously dried and weighed filter
sediment to the nearest 0.01 % m/m. For each test specimen
media on top of the sinter support with the mesh imprint side
with a total sediment concentration ≤0.005 % m/m, record the
down, using forceps. Apply slight vacuum to aid in centering
result as 0.00 % m/m.
the filter media, and place the top portion of the filtration
apparatus carefully on to the media before clamping. Shut off
M 2 M 2 M 2 M
~ ! ~ !
5 4 3 2
S 5 (1)
the vacuum and pass steam at 100 6 1°C through the
10 M
heating/cooling coils for 10 min prior to sample addition.
where:
9.4 Sample Addition—Into a 30 mL beaker, pour approxi-
S = total sediment, % m/m,
mately 11 g of the fuel sample prepared as described in 9.1 and
M = mass of sample, g,
weigh to the nearest 0.01 g. Connect the vacuum source and
M = mass of lower filter medium before filtration, mg,
apply vacuum to an absolute pressure of 40 6 2 kPa minimum
M = mass of lower filter medium after filtration, mg,
(61.3 kPa vacuum). Heat the contents of the beaker to 100 6
M = mass of upper filter medium before filtration, mg, and
2°C. Then transfer the contents at 100 6 2°C (Note 3)tothe
M = mass of upper filter medium after filtration, mg.
center of the filter medium, taking care that no sample touches
11. Report
the walls during transfer (Note 4). Reweigh the beaker to the
nearest 0.01 g. The quantity transferred should be 106 0.5 g.
11.1 Report the total sediment by hot filtration as the
When filtration is not complete in 25 min, discontinue the test
average of duplicate determinations, to the nearest 0.01 %
and repeat using 5 6 0.3 g of sample. If filtration is still not
m⁄m. If the average of the duplicate determinations is <0.01 %
complete in 25 min, report the result as filtration exceeds 25
m/m, report it as “<0.01 % m/m.” If a 5-g sample has been
min.
used, report the results as total sediment (5 g) by hot filtration.
If filtration is not complete within the specified 25 min, report
NOTE 3—It is expedient to weigh the beaker plus stirrer plus tempera-
ture measurement device before and after transfer to avoid errors incurred the results as filtration time exceeds 25 min.
byattemptingtoobtainanetweight.Anyconvenientmeansofheatingthe
11.2 Test Report—The test report shall contain at least the
fuel sample to 1006 2°C may be used, such as hot plate, water or oil bath,
following information:
or an oven when equipped with a suitable stirrer. Samples that overheat
above 105°C must be discarded and not reused. 11.2.1 The type and identification of the product tested,
D4870 − 09 (2014)
11.2.2 A reference to this test method,
r 5 0.048 =x for distillate fuels containing (3)
11.2.3 The result of the test (see 11.1),
11.2.4 Any deviation, by agreement or otherwise, from the residual components
standard procedures specified (see 11.1), and
where x = the average of the test results, % m/m.
11.2.5 The date of the test.
12.1.2 Reproducibility—The difference between two test
results, expressed as the average of duplicate determinations
12. Precision and Bias
independently obtained by different operators operating in
12.1 Precision—The precision of this test method as deter-
different laboratories on nominally identical test material
mined by the statistical examination of interlaboratory test
would, in the long run, in the normal and correct operation of
results is as follows. The results ranged from 0.01 to 0.40 %
the test method, exceed the following values only one case in
m/m for distillate fuel oils containing residual components and
twenty:
from 0.01 to 0.50 % m/m for residual fuel oils.
R 5 0.294=x for residual fuels, and (4)
12.1.1 Repeatability—The difference between successive
test results, expressed as the average of duplicate
R 5 0.174 =x for distillate fuels containing (5)
determinations, obtained by the same operator with the same
apparatus under constant operating conditions on identical test residual components
material, would, in the long run, in the normal and correct
where x = the average of the test results, % m/m.
operation of the test method, exceed the following values only
12.2 Bias—Since there is no accepted reference material
in one case in twenty:
suitable for determining the bias for the procedure in this test
r 5 0.089 =x for residual fuels, and (2)
method, bias cannot be determined.
13. Keywords
4 13.1 ageing; fuel oils; hot filtration; residual fuel; sediment;
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1238. storage stability; total sediment
ANNEX
(Mandatory Information)
A1. HAZARD STATEMENTS
A1.1 n-Heptane A1.2 Toluene
A1.1.1 Keep away from heat, sparks, and open flame. A1.2.1 Keep away from heat, sparks, and open flame.
Keep container closed. Keep container closed.
Use with adequate ventilation. Use with adequate ventilation.
Avoid prolonged breathing of vapor or spray mist. Avoid breathing of vapor or spray mist.
Avoid prolonged or repeated skin contact. Avoid prolonged or repeated skin contact.
APPENDIX
(Nonmandatory Information)
X1. PREDICTION OF TOTAL SEDIMENT IN RESIDUAL FUEL
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D4870 − 09 D4870 − 09 (Reapproved 2014)
Designation: 375/99
Standard Test Method for
Determination of Total Sediment in Residual Fuels
This standard is issued under the fixed designation D4870; 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.
1. Scope*Scope
1.1 This test method covers the determination of total sediment up to 0.40 % m/m for distillate fuel oils containing residual
components and to 0.50 % m/m in residual fuel oils having a maximum viscosity of 55 cSt (mm /s) at 100°C. Some fuels can
exceed the maximum filtration time specified in this test method due to factors other than the presence of significant quantities of
insoluble organic or inorganic material. This test method can be used for the assessment of total sediment after regimes of fuel
pretreatment designed to accelerate the aging process.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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 and health practices and determine the applicability of regulatory
limitations prior to use. For specific warning statements, see 7.2, 7.3, Annex A1, and X1.6.1.
2. Referenced Documents
2.1 ASTM Standards:
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
E1 Specification for ASTM Liquid-in-Glass Thermometers
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 total sediment—the sum of the insoluble organic and inorganic material that is separated from the bulk of the residual fuel
oil by filtration through a Whatman GF/A filter medium, and that is also insoluble in a predominantly paraffinic solvent.
4. Summary of Test Method
4.1 A weighed quantity (10 g) of the oil sample is filtered through the prescribed apparatus at 100°C. After solvent washing and
drying the total sediment on the filter medium is weighed. The test is to be carried out in duplicate.
5. Significance and Use
5.1 Appreciable amounts of sediment in a residual fuel oil can cause fouling of facilities for handling, and give problems in
burner mechanisms. Sediment can accumulate in storage tanks, on filter screens, or on burner parts, resulting in obstruction of the
flow of oil from the tank to the burner.
6. Apparatus
6.1 Filtration Apparatus, constructed of brass, with copper steam coils attached, suitably supported above a vacuum flask
appropriately protected against the effects of implosion. See Figs. 1 and 2.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.14 on Stability and Cleanliness of Liquid Fuels.
Current edition approved April 15, 2009Dec. 1, 2014. Published May 2009February 2015. Originally approved in 1988. Last previous edition approved in 20072009 as
D4870D4870 – 09.–07a. DOI: 10.1520/D4870-09.10.1520/D4870-09R14.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*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
D4870 − 09 (2014)
FIG. 1 Detail of Filtration Cell
FIG. 2 Arrangement of Filtration Apparatus
6.2 Temperature Measuring Device , capable of measuring the temperature in the range from 95 to 105°C with an accuracy of
0.5°C.
6.3 Oven, electric, capable of maintaining a temperature of 110 6 1°C. The oven should be capable of safely evaporating the
solvent without risk of fire.
6.4 Stirring Rod, glass or polytetrafluoroethylene (PTFE) approximately 150 mm in length and 3 mm in diameter.
6.5 Beaker, glass, 30 mL capacity, either squat form with lip or conical.
6.6 Small Dishes, such as watch glasses or Petri dishes.
6.7 Hotplate, electric.
6.8 Steam Generator, to provide steam at 100 6 1°C.
6.9 Vacuum Source, capable of providing the specified vacuum.
D4870 − 09 (2014)
6.10 Vacuum Gauge, capable of measuring the specified vacuum.
6.11 Filter Medium, Whatman glass fiber filter medium, Grade GF/A, 47 mm diameter.
6.12 High Speed Mixer, any convenient type, minimum speed 400 rpm.
6.13 Desiccator.
6.14 Cooling Vessel, a desiccator or other type of tightly covered vessel for cooling the filter media before weighing. The use
of a drying agent is not recommended.
6.15 Syringe or Graduated Wash Bottle , minimum capacity 25 mL, graduated in 0.5 mL increments.
6.16 Forceps, spade-ended.
7. Reagents and Materials
7.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the committee on Analytical Reagents of the American Chemical Society, where
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
7.2 Normal Heptane, minimum 99.75 % purity. (Warning—Flammable, vapor harmful if inhaled. See A1.1.)
7.3 Toluene, at least reagent grade purity. (Warning—Flammable, vapor harmful. See A1.2. )
7.4 Wash Solvent, consisting of 85 volume % n-heptane (7.2) and 15 volume % toluene (see 7.3).
8. Sampling
8.1 Sample in accordance with Practice D4057 or Practice D4177.
9. Procedure
9.1 Sample Preparation—Mix the whole sample, as received, thoroughly using a high speed mixer when practicable, for 30 s.
In all cases a sample taken on a glass or PTFE rod dipped to the bottom of the container must show a homogeneous appearance.
For fuels with a high wax content (high pour point), or of very high viscosity, the sample must be heated before stirring. The
temperature must be either 15°C above the pour point in the case of low viscosity fuels, or that equivalent to 150 to 250 cSt in
the case of high viscosity fuels. In no case should the temperature exceed 80°C.
9.2 Filter Preparation—For each test, dry two filter media for 20 min in the oven at 110°C. Transfer each filter medium,
separately, rapidly to a cooling vessel and allow to cool to room temperature for 20 min. Weigh each filter medium to the nearest
0.0001 g.
NOTE 1—The Whatman GF/A filter media are fragile and are to be handled with care. Before use, check each medium for consistency, and the possible
presence of small defects (holes).
NOTE 2—For convenience, place the filters on numbered small dishes (6.6) during drying and cooling.
9.3 Apparatus Assembly—Before use, check that the filter support screen is clean. If necessary, the screen must be cleaned by
boiling in a high boiling point aromatic solvent. When more than 2 % of the sinter area remains blocked by particulate matter after
such cleaning, discard the screen and install a new one.
9.3.1 The filtration unit must be clean and dry before assembly. Stack the two previously dried and weighed filter media on top
of the sinter support with the mesh imprint side down, using forceps. Apply slight vacuum to aid in centering the filter media, and
place the top portion of the filtration apparatus carefully on to the media before clamping. Shut off the vacuum and pass steam at
100 6 1°C through the heating/cooling coils for 10 min prior to sample addition.
9.4 Sample Addition—Into a 30 mL beaker, pour approximately 11 g of the fuel sample prepared as described in 9.1 and weigh
to the nearest 0.01 g. Connect the vacuum source and apply vacuum to an absolute pressure of 40 6 2 kPa minimum (61.3 kPa
vacuum). Heat the contents of the beaker to 100 6 2°C. Then transfer the contents at 100 6 2°C (Note 3) to the center of the filter
medium, taking care that no sample touches the walls during transfer (Note 4). Reweigh the beaker to the nearest 0.01 g. The
quantity transferred should be 106 0.5 g. When filtration is not complete in 25 min, discontinue the test and repeat using 5 6 0.3
g of sample. If filtration is still not complete in 25 min, report the result as filtration exceeds 25 min.
NOTE 3—It is expedient to weigh the beaker plus stirrer plus temperature measurement device before and after transfer to avoid errors incurred by
attempting to obtain a net weight. Any convenient means of heating the fuel sample to 1006 2°C may be used, such as hot plate, water or oil bath, or
an oven when equipped with a suitable stirrer. Samples that overheat above 105°C must be discarded and not reused.
NOTE 4—For samples of high viscosity or high sediment, level filtration will be aided by small stage or even dropwise addition. It is preferable to avoid
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed by
the American Chemical Society, see Annual Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
D4870 − 09 (2014)
complete coverage of the filter medium with unfiltered oil sample. For samples of low filtration rate the pressure of 40 6 2 kPa should be maintained
for the 25-min period.
9.5 Filter Washing—When the filtration is complete and the upper filter medium appears dry, continue the steam and vacuum
for a further 5 min. Discontinue the steam supply and cool the apparatus by passing tap water through the coils. Wash the filtration
unit carefully with two portions of 25 6 1 mL of the wash solvent from a syringe or graduated wash bottle with a fine nozzle, taking
care to remove any adhered sample from the wall of the upper part of the apparatus. Carefully remove the top portion of the
filtration unit and wash the rim of the filter with a further 10 6 0.5 mL of the wash solvent in a similar manner. Finally wash the
whole of the filter medium area with 10 6 0.5 mL of n-heptane.
NOTE 5—If the sample filters very rapidly, the vacuum should be released before the first solvent washing, to ensure complete coverage of the filter
medium area by solvent. The vacuum should then be gently reapplied for the subsequent operations.
9.6 Apparatus Disassembly—After the filter medium appears dry, discontinue the vacuum supply. Using the forceps, carefully
remove each filter medium separately and transfer them to the oven at 110°C. Dry for 20 min and quickly transfer them to the
cooling vessel (6.14). Allow them to cool to room temperature for 20 min and reweigh them to the nearest 0.0001 g.
10. Calculation
10.1 Calculate the mass percentage of total sediment for each test specimen using Eq 1. For each test specimen with a calculated
total sediment concentration >0.005 % m/m as determined by Eq 1, record the mass percentage of total sediment to the nearest
0.01 % m/m. For each test specimen with a total sediment concentration ≤0.005 % m/m, record the result as 0.00 % m/m.
M 2 M 2 M 2 M
~ ! ~ !
5 4 3 2
S 5 (1)
10 M
where:
S = total sediment, % m/m,
M = mass of sample, g,
M = mass of lower filter medium before filtration, mg,
M = mass of lower filter medium after filtration, mg,
M = mass of upper filter medium before filtration, mg, and
M = mass of upper filter medium after filtration, mg.
11. Report
11.1 Report the total sediment by hot filtration as the average of duplicate determinations, to the nearest 0.01 % m ⁄m. If the
average of the duplicate determinations is <0.01 % m/m, report it as “<0.01 % m/m.” If a 5-g sample has been used, report the
results as total sediment (5 g) by hot filtration. If filtration is not complete within the specified 25 min, report the results as filtration
time exceeds 25 min.
11.2 Test Report—The test report shall contain at least the following information:
11.2.1 The type and identification of the product tested,
11.2.2 A reference to this test method,
11.2.3 The result of the test (see 11.1),
11.2.4 Any deviation, by agreement or otherwise, from the standard procedures specified (see 11.1), and
11.2.5 The date of the test.
12. Precision and Bias
12.1 Precision—The precision of this test method as determined by the statistical examination of interlaboratory test results is
as follows. The results ranged from 0.01 to 0.40 % m/m for distillate fuel oils containing residual components and from 0.01 to
0.50 % m/m for residual fuel oils.
12.1.1 Repeatability—The difference between successive test results, expressed as the average of duplicate determinations,
obtained by the same operator with the same apparatus under constant operating conditions on identical test material, would, in
the long run, in the normal and correct operation of the test method, exceed the following values only in one case in twenty:
=
r 5 0.089 x for residual fuels, and (2)
r 5 0.048 =x for distillate fuels containing (3)
residual components
where x = the average of the test results, % m/m.
Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1238.
D4870 − 09 (2014)
12.1.2 Reproducibility—The difference between two test results, expressed as the average of duplicate determinations
independently obtained by different operators operating in different laboratories on nominally identical test material would, in the
long run, in the normal and correct operation of the test method, exceed the following values only one case in twenty:
R 5 0.294=x for residual fuels, and (4)
R 5 0.174 =x for distillate fuels containing (5)
residual components
where x = the average of the test results, % m/m.
12.2 Bias—Since there is no accepted reference material suitable for determining the bias for the procedure in this test method,
bias cannot be determined.
13. Keywords
13.1 ageing; fuel oils; hot filtration; residual fuel; sediment; storage stability; tota
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.