ASTM D4870-22

• Abstract:

  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, health, and environmental 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. ; 1.4 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.

• Status: Published
• Publication Date: 30-Nov-2022
• ICS: 75.160.20 - Liquid fuels
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.14 - Stability, Cleanliness and Compatibility of Liquid Fuels

• Refers: ASTM D4175-23a - Standard Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
• Effective Date: 15-Dec-2023
• Refers: ASTM D4175-23e1 - Standard Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
• Effective Date: 01-Jul-2023
• Refers: ASTM E1-13 - Standard Specification for ASTM Liquid-in-Glass Thermometers
• Effective Date: 01-May-2013
• Refers: ASTM D4057-06(2011) - Standard Practice for Manual Sampling of Petroleum and Petroleum Products
• Effective Date: 01-Jun-2011
• Refers: ASTM E1-07 - Standard Specification for ASTM Liquid-in-Glass Thermometers
• Effective Date: 01-Nov-2007
• Refers: ASTM E1-05 - Standard Specification for ASTM Liquid-in-Glass Thermometers
• Effective Date: 01-Nov-2005
• Refers: ASTM E1-03a - Standard Specification for ASTM Liquid-in-Glass Thermometers
• Effective Date: 01-Nov-2003
• Refers: ASTM E1-03 - Standard Specification for ASTM Thermometers
• Effective Date: 10-May-2003
• Refers: ASTM E1-01 - Standard Specification for ASTM Thermometers
• Effective Date: 10-Oct-2001
• Refers: ASTM E1-98e1 - Standard Specification for ASTM Thermometers
• Effective Date: 10-Oct-2001
• Refers: ASTM E1-98 - Standard Specification for ASTM Thermometers
• Effective Date: 10-Oct-2001
• Refers: ASTM D4057-95(2000) - Standard Practice for Manual Sampling of Petroleum and Petroleum Products
• Effective Date: 10-Apr-2000

Overview

ASTM D4870-22 is the Standard Test Method for Determination of Total Sediment in Residual Fuels, developed by ASTM International. This standard defines procedures for quantifying the total content of insoluble organic and inorganic sediments in residual fuel oils and distillate blends. Managing sediment levels is essential for the stability, storage, and reliable operation of heavy fuel systems. This method provides valuable data for fuel suppliers, operators, and laboratories to assess potential operational issues related to sediment accumulation.

Key Topics

• Total Sediment Determination: Measures insoluble materials filtered from residual fuel oils using a hot filtration method.
• Applicability: Covers distillate fuel oils containing residual components (up to 0.40% m/m) and residual fuels with viscosities up to 55 cSt at 100°C (up to 0.50% m/m sediment).
• Storage and Handling Problems: High sediment levels can foul storage tanks, block filter screens, and damage burner mechanisms, leading to restricted fuel flow and system inefficiency.
• Aging Assessment: The method enables evaluation of total sediment after accelerated aging processes so that storage stability can be predicted.
• Precision and Reporting: Results are reported as an average, with repeatability and reproducibility metrics for quality control.
• Safety and Compliance: Users must follow appropriate safety, health, and environmental guidelines, considering hazards of solvents used (such as n-heptane and toluene).

Applications

The determination of total sediment in residual fuels is critical for:

• Quality Control: Ensuring that heavy fuel oils meet specified sediment limits before dispensing or use.
• Fuel Storage Management: Identifying fuels that are likely to form problematic deposits during storage, facilitating proactive measures.
• Operational Reliability: Maintaining clean burner nozzles and filter screens to prevent flow obstructions and equipment failures in power plants, marine engines, and industrial boilers.
• Predictive Maintenance: Using the standard's accelerated aging regimes to predict future sediment formation and storage stability, minimizing downtime and unplanned maintenance.
• Regulatory Compliance: Meeting industry and contractual specifications regarding sediment levels in supplied residual fuels.

Related Standards

ASTM D4870-22 references and aligns with several related ASTM and international standards:

• ASTM D4057 – Practice for Manual Sampling of Petroleum and Petroleum Products
• ASTM D4175 – Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
• ASTM D4177 – Practice for Automatic Sampling of Petroleum and Petroleum Products
• ASTM E1 – Specification for ASTM Liquid-in-Glass Thermometers

The test method is also technically equivalent to relevant standards developed by the Energy Institute in London, promoting harmonization across international fuel quality assessments.

---

By adhering to ASTM D4870-22, organizations achieve a consistent, reliable approach to identifying and mitigating the operational risks associated with sediment in residual fuel oils. This enhances equipment longevity, supports safety in fuel handling, and ensures compliance with global fuel quality standards.

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: D4870 − 22
Designation: 375/11 (2021) and 390/11 (2017)
Standard Test Method for
1,2
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* 2. Referenced Documents
1.1 This test method covers the determination of total 2.1 ASTM Standards:
sediment up to 0.40 % m/m for distillate fuel oils containing D4057 Practice for Manual Sampling of Petroleum and
residual components and to 0.50 % m/m in residual fuel oils Petroleum Products
having a maximum viscosity of 55 cSt (mm /s) at 100 °C. D4175 Terminology Relating to Petroleum Products, Liquid
Somefuelscanexceedthemaximumfiltrationtimespecifiedin Fuels, and Lubricants
this test method due to factors other than the presence of D4177 Practice for Automatic Sampling of Petroleum and
significantquantitiesofinsolubleorganicorinorganicmaterial. Petroleum Products
This test method can be used for the assessment of total E1 Specification for ASTM Liquid-in-Glass Thermometers
sediment after regimes of fuel pretreatment designed to accel-
3. Terminology
erate the aging process.
3.1 Definitions:
1.2 The values stated in SI units are to be regarded as
3.1.1 For definitions of terms used in this test method, refer
standard. No other units of measurement are included in this
to Terminology D4175.
standard.
3.2 Definitions of Terms Specific to This Standard:
1.3 This standard does not purport to address all of the
3.2.1 total sediment, n—the sum of the insoluble organic
safety concerns, if any, associated with its use. It is the
and inorganic material that is separated from the bulk of the
responsibility of the user of this standard to establish appro-
residual fuel oil by filtration through a Whatman GF/A filter
priate safety, health, and environmental practices and deter-
medium, and that is also insoluble in a predominantly paraf-
mine the applicability of regulatory limitations prior to use.
finic solvent.
For specific warning statements, see 7.2, 7.3, Annex A1, and
X1.6.1.
4. Summary of Test Method
1.4 This international standard was developed in accor-
4.1 A weighed quantity (10 g) of the oil sample is filtered
dance with internationally recognized principles on standard-
through the prescribed apparatus at 100 °C. After solvent
ization established in the Decision on Principles for the
washing and drying the total sediment on the filter medium is
Development of International Standards, Guides and Recom-
weighed. The test is to be carried out in duplicate.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
5. Significance and Use
5.1 Appreciable amounts of sediment in a residual fuel oil
This test method is under the jurisdiction of ASTM International Committee
can cause fouling of facilities for handling, and give problems
D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct
responsibility of ASTM Subcommittee D02.14 on Stability, Cleanliness and in burner mechanisms. Sediment can accumulate in storage
Compatibility of Liquid Fuels. The technically equivalent standard as referenced is
tanks, on filter screens, or on burner parts, resulting in
under the jurisdiction of the Energy Institute Subcommittee SC-B-5.
obstruction of the flow of oil from the tank to the burner.
Current edition approved Dec. 1, 2022. Published December 2022. Originally
approved in 1988. Last previous edition approved in 2018 as D4870 – 18. DOI:
10.1520/D4870-22.
2 3
This test method has been developed through the cooperative effort between For referenced ASTM standards, visit the ASTM website, www.astm.org, or
ASTM and the Energy Institute, London.ASTM and IPstandards were approved by contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
ASTMandEItechnicalcommitteesasbeingtechnicallyequivalentbutthatdoesnot Standards volume information, refer to the standard’s Document Summary page on
imply both standards are identical. 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 − 22
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.
6.2 Temperature Measuring Device, capable of measuring
the temperature in the range from 95 °C to 105 °C with an
accuracy of 0.5 °C.
6.3 Oven, electric, capable of maintaining a temperature of
110 °C 6 1 °C. The oven should be capable of safely evapo-
rating the solvent without risk of fire.
6.4 Stirring Rod, glass or polytetrafluoroethylene (PTFE) FIG. 2 Arrangement of Filtration Apparatus
approximately 150 mm in length and 3 mm in diameter.
6.5 Beaker, glass, 30 mLcapacity, either squat form with lip
or conical.
6.11 Filter Medium, Whatman glass fiber filter medium,
6.6 Small Dishes, such as watch glasses or Petri dishes.
Grade GF/A, 47 mm diameter.
6.7 Hotplate, electric.
6.12 High Speed Mixer, any convenient type, minimum
6.8 Steam Generator, to provide steam at 100 °C 6 1 °C. speed 400 r⁄min.
6.9 Vacuum Source, capable of providing the specified 6.13 Desiccator.
vacuum.
6.14 Cooling Vessel, a desiccator or other type of tightly
6.10 Vacuum Gauge, capable of measuring the specified covered vessel for cooling the filter media before weighing.
vacuum. The use of a drying agent is not recommended.
FIG. 1 Detail of Filtration Cell
D4870 − 22
6.15 Syringe or Graduated Wash Bottle, minimum capacity 9.3.1 The filtration unit must be clean and dry before
25 mL, graduated in 0.5 mL increments. assembly. Stack the two previously dried and weighed filter
media on top of the sinter support with the mesh imprint side
6.16 Forceps, spade-ended.
down, using forceps. Apply slight vacuum to aid in centering
7. Reagents and Materials the filter media, and place the top portion of the filtration
apparatus carefully on to the media before clamping. Shut off
7.1 Purity of Reagents—Reagent grade chemicals shall be
the vacuum and pass steam at 100 °C 6 1 °C through the
used in all tests. Unless otherwise indicated, it is intended that
heating/cooling coils for 10 min prior to sample addition.
all reagents shall conform to the specifications of the commit-
tee onAnalytical Reagents of theAmerican Chemical Society, 9.4 Sample Addition—Into a 30 mL beaker, pour approxi-
where such specifications are available. Other grades may be mately 11 g of the fuel sample prepared as described in 9.1 and
used, provided it is first ascertained that the reagent is of weigh to the nearest 0.01 g. Connect the vacuum source and
sufficiently high purity to permit its use without lessening the
apply vacuum to an absolute pressure of 40 kPa 6 2 kPa
accuracy of the determination. minimum (61.3 kPa vacuum). Heat the contents of the beaker
to 100 °C 6 2 °C. Then transfer the contents at 100 °C 62°C
7.2 Normal Heptane, minimum 99.75 % purity.
(Note 3) to the center of the filter medium, taking care that no
(Warning—Flammable, vapor harmful if inhaled. See A1.1.)
sample touches the walls during transfer (Note 4). Reweigh the
7.3 Toluene, at least reagent grade purity. (Warning—
beaker to the nearest 0.01 g.The quantity transferred should be
Flammable, vapor harmful. See A1.2.)
10 g 6 0.5 g. When filtration is not complete in 25 min,
7.4 Wash Solvent, consisting of 85 % by volume n-heptane discontinue the test and repeat using 5 g 6 0.3 g of sample. If
filtration is still not complete in 25 min, report the result as
(7.2) and 15 % by volume toluene (see 7.3).
filtration exceeds 25 min.
8. Sampling
NOTE 3—It is expedient to weigh the beaker plus stirrer plus tempera-
8.1 Sample in accordance with Practice D4057 or Practice
ture measurement device before and after transfer to avoid errors incurred
D4177. byattemptingtoobtainanetweight.Anyconvenientmeansofheatingthe
fuel sample to 100 °C 6 2 °C may be used, such as hot plate, water or oil
9. Procedure
bath, or an oven when equipped with a suitable stirrer. Samples that
overheat above 105 °C must be discarded and not reused.
9.1 Sample Preparation—Mix the whole sample, as
NOTE4—Forsamplesofhighviscosityorhighsediment,levelfiltration
received, thoroughly using a high speed mixer when
will be aided by small stage or even dropwise addition. It is preferable to
practicable, for 30 s. In all cases a sample taken on a glass or avoid complete coverage of the filter medium with unfiltered oil sample.
For samples of low filtration rate the pressure of 40 kPa 6 2 kPa should
PTFE rod dipped to the bottom of the container must show a
be maintained for the 25 min period.
homogeneous appearance. For fuels with a high wax content
(high pour point), or of very high viscosity, the sample must be 9.5 Filter Washing—When the filtration is complete and the
upper filter medium appears dry, continue the steam and
heated before stirring. The temperature must be either 15 °C
vacuum for a further 5 min. Discontinue the steam supply and
above the pour point in the case of low viscosity fuels, or that
cooltheapparatusbypassingtapwaterthroughthecoils.Wash
equivalent to 150 cSt to 250 cSt in the case of high viscosity
the filtration unit carefully with two portions of 25 mL 61mL
fuels. In no case should the temperature exceed 80 °C.
of the wash solvent from a syringe or graduated wash bottle
9.2 Filter Preparation—For each test, dry two filter media
with a fine nozzle, taking care to remove any adhered sample
for 20 min in the oven at 110 °C. Transfer each filter medium,
from the wall of the upper part of the apparatus. Carefully
separately, rapidly to a cooling vessel and allow to cool to
remove the top portion of the filtration unit and wash the rim
room temperature for 20 min. Weigh each filter medium to the
of the filter with a further 10 mL 6 0.5 mLof the wash solvent
nearest 0.0001 g.
in a similar manner. Finally wash the whole of the filter
NOTE 1—The Whatman GF/A filter media are fragile and are to be
medium area with 10 mL 6 0.5 mL of n-heptane.
handled with care. Before use, check each medium for consistency, and
NOTE 5—If the sample filters very rapidly, the vacuum should be
the possible presence of small defects (holes).
NOTE 2—For convenience, place the filters on numbered small dishes released before the first solvent washing, to ensure complete coverage of
the filter medium area by solvent. The vacuum should then be gently
(6.6) during drying and cooling.
reapplied for the subsequent operations.
9.3 Apparatus Assembly—Before use, check that the filter
9.6 Apparatus Disassembly—After the filter medium ap-
support screen is clean. If necessary, the screen must be
pears dry, discontinue the vacuum supply. Using the forceps,
cleaned by boiling in a high boiling point aromatic solvent.
carefully remove each filter medium separately and transfer
When more than 2 % of the sinter area remains blocked by
themtotheovenat110 °C.Dryfor20 minandquicklytransfer
particulate matter after such cleaning, discard the screen and
them to the cooling vessel (6.14). Allow them to cool to room
install a new one.
temperature for 20 min and reweigh them to the nearest
0.0001 g.
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
Standard-Grade Reference Materials, American Chemical Society, Washington,
DC. For suggestions on the testing of reagents not listed by theAmerican Chemical 10. Calculation
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
10.1 Calculate the mass percentage of total sediment for
U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
copeial Convention, Inc. (USPC), Rockville, MD. each test specimen using Eq 1. For each test specimen with a
D4870 − 22
calculated total sediment concentration >0.005 % m/m as results is as follows. The results ranged from 0.01 % to 0.40 %
determined by Eq 1, record the mass percentage of total m/m for distillate fuel oils containing residual components and
sediment to the nearest 0.01 % m⁄m. For each test specimen
from 0.01 % to 0.50 % m⁄m for residual fuel oils.
with a total sediment concentration ≤0.005 % m⁄m, record the
12.1.1 Repeatability—The difference between successive
result as 0.00 % m/m.
test results, expressed as the average of duplicate
M 2 M 2 M 2 M
determinations, obtained by the same operator with the same
~ ! ~ !
5 4 3 2
S 5 (1)
10 M apparatus under constant operating conditions on identical test
material, would, in the long run, in the normal and correct
where:
operation of the test method, exceed the following values only
S = total sediment, percent m/m,
in one case in twenty:
M = mass of sample, g,
M = mass of lower filter medium before filtration, mg,
r 5 0.089 =x for residual fuels, and (2)
M = mass of lower filter medium after filtration, mg,
=
M = mass of upper filter medium before filtration, mg, and r 5 0.048 x for distillate fuels containing (3)
M = mass of upper filter medium after filtration, mg.
residual components
11. Report
where x = the average of the test results, % m/m.
11.1 Report the total sediment by hot filtration as the
12.1.2 Reproducibility—The difference between two test
average of duplicate determinations, to the nearest 0.01 %
results, expressed as the average of duplicate determinations
m⁄m. If the average of the duplicate determinations is <0.01 %
independently obtained by different operators operating in
m⁄m, report it as “<0.01 % m/m.” If a 5 g sample has been
different laboratories on nominally identical test material
used, report the results as total sediment (5 g) by hot filtration.
If filtration is not complete within the specified 25 min, report would, in the long run, in the normal and correct operation of
the results as filtration time exceeds 25 min. the test method, exceed the following values only one case in
twenty:
11.2 Test Report—The test report shall contain at least the
following information:
R 5 0.294=x for residual fuels, and (4)
11.2.1 The type and identification of the product tested,
=
11.2.2 A reference to this test method, R 5 0.174 x for distillate fuels containing (5)
11.2.3 The result of the test (see 11.1),
residual components
11.2.4 Any deviation, by agreement or otherwise, from the
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.
12.2 Bias—Since there is no accepted reference material
12. Precision and Bias
suitable for determining the bias for the procedure in this test
12.1 Precision—The precision of this test method as deter-
method, bias cannot be determined.
mined by the statistical examination of interlaboratory test
13. Keywords
Supporting data have been filed at ASTM Internationa
...

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 − 18 D4870 − 22
Designation: 375/99375/11 (2021) and 390/11 (2017)
Standard Test Method for
1,2
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*
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, health, and environmental 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.
1.4 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.
2. Referenced Documents
2.1 ASTM Standards:
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
E1 Specification for ASTM Liquid-in-Glass Thermometers
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this test method, refer to Terminology D4175.
3.2 Definitions of Terms Specific to This Standard:
This test method is under the jurisdiction of ASTM International Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility
of ASTM Subcommittee D02.14 on Stability, Cleanliness and Compatibility of Liquid Fuels. The technically equivalent standard as referenced is under the jurisdiction of
the Energy Institute Subcommittee SC-B-5.
Current edition approved April 1, 2018Dec. 1, 2022. Published May 2018December 2022. Originally approved in 1988. Last previous edition approved in 20142018 as
D4870 – 09 (2014).D4870 – 18. DOI: 10.1520/D4870-18.10.1520/D4870-22.
This test method has been developed through the cooperative effort between ASTM and the Energy Institute, London. ASTM and IP standards were approved by ASTM
and EI technical committees as being technically equivalent but that does not imply both standards are identical.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. 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 − 22
3.2.1 total sediment, n—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.
6.2 Temperature Measuring Device, capable of measuring the temperature in the range from 95 °C to 105 °C with an accuracy
of 0.5 °C.
6.3 Oven, electric, capable of maintaining a temperature of 110 °C 6 1 °C. The oven should be capable of safely evaporating the
solvent without risk of fire.
FIG. 1 Detail of Filtration Cell
D4870 − 22
FIG. 2 Arrangement of Filtration Apparatus
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 °C 6 1 °C.
6.9 Vacuum Source, capable of providing the specified vacuum.
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 r ⁄min.
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.
Reagent Chemicals, American Chemical Society Specifications,ACS Reagent Chemicals, Specifications and Procedures for Reagents and Standard-Grade Reference
Materials, American Chemical Society, Washington, DC. For Suggestionssuggestions on the testing of reagents not listed by the American Chemical Society, see
AnnualAnalar 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 − 22
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 % by volume n-heptane (7.2) and 15 % by 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 cSt 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 °C 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 kPa 6 2 kPa minimum (61.3 kPa
vacuum). Heat the contents of the beaker to 100 °C 6 2 °C. Then transfer the contents at 100 °C 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 10 g 6 0.5 g. When filtration is not complete in 25 min, discontinue the test and repeat
using 5 g 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 100 °C 6 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
complete coverage of the filter medium with unfiltered oil sample. For samples of low filtration rate the pressure of 40 kPa 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 mL 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
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the filtration unit and wash the rim of the filter with a further 10 mL 6 0.5 mL of the wash solvent in a similar manner. Finally
wash the whole of the filter medium area with 10 mL 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, percent 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:
Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1238. Contact ASTM Customer
Service at [e-mail].
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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.
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 refere
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