ASTM D4870-99
(Test Method)Standard Test Method for Determination of Total Sediment in Residual Fuels
Standard Test Method for Determination of Total Sediment in Residual Fuels
SCOPE
1.1 This test method covers the determination of total sediment up to 0.40% m/m in residual fuel oils having a maximum viscosity of 55 cST (mm 2/S) at 100C. 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 acceptable SI units are to be regarded as the 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 hazard statements see Note 1, Note 2, and Annex A1.
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An American National Standard
Designation: D 4870 – 99
Designation: 375/99
Standard Test Method for
Determination of Total Sediment in Residual Fuels
This standard is issued under the fixed designation D 4870; 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 (e) indicates an editorial change since the last revision or reapproval.
This test method has been approved by the sponsoring committees and accepted by the cooperating societies in accordance with
established procedures.
1. Scope 3. Terminology
1.1 This test method covers the determination of total 3.1 Definitions of Terms Specific to This Standard:
sediment up to 0.40 % m/m for distillate fuel oils containing 3.1.1 total sediment—the sum of the insoluble organic and
residual components and to 0.50 % m/m in residual fuel oils inorganic material that is separated from the bulk of the
having a maximum viscosity of 55 cSt (mm /s) at 100°C. Some residual fuel oil by filtration through a Whatman GF/A filter
fuels can exceed the maximum filtration time specified in this medium, and that is also insoluble in a predominantly paraf-
test method due to factors other than the presence of significant finic solvent.
quantities of insoluble organic or inorganic material. This test
4. Summary of Test Method
method can be used for the assessment of total sediment after
regimes of fuel pretreatment designed to accelerate the aging 4.1 A weighed quantity (10 g) of the oil sample is filtered
through the prescribed apparatus at 100°C. After solvent
process.
1.2 The values stated in acceptable SI units are to be washing and drying the total sediment on the filter medium is
weighed. The test is to be carried out in duplicate.
regarded as the standard.
1.3 This standard does not purport to address all of the
5. Significance and Use
safety concerns, if any, associated with its use. It is the
5.1 Appreciable amounts of sediment in a residual fuel oil
responsibility of the user of this standard to establish appro-
can cause fouling of facilities for handling, and give problems
priate safety and health practices and determine the applica-
in burner mechanisms. Sediment can accumulate in storage
bility of regulatory limitations prior to use. For specific hazard
tanks, on filter screens, or on burner parts, resulting in
statements see Note 1, Note 2, and Annex A1.
obstruction of the flow of oil from the tank to the burner.
2. Referenced Documents
6. Apparatus
2.1 ASTM Standards:
6.1 Filtration Apparatus, constructed of brass, with copper
D 362 Specification for Industrial Grade Toluene
steam coils attached, suitably supported above a vacuum flask
D 2880 Specification for Gas Turbine Fuel Oils
appropriately protected against the effects of implosion. See
D 4057 Practice for Manual Sampling of Petroleum and
Figs. 1 and 2.
Petroleum Products
6.2 Thermometer, partial immersion type ranging from
D 4177 Practice for Automatic Sampling of Petroleum and
approximately 95 to 103°C. Maximum length 220 mm. Maxi-
Petroleum Products
mum graduation interval 0.5°C.
E 1 Specification for ASTM Thermometers
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.
This test method is under the jurisdiction of ASTM Committee D02 on
6.4 Stirring Rod, glass or PTFE approximately 150 by 3 mm
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
diameter.
D02.14 on Stability and Cleanliness of Liquid Fuels.
Current edition approved June 10, 1999. Published August 1999. Originally
6.5 Beaker, glass, 30 mL capacity, either squat form with lip
published as D 4870 – 88. Last previous edition D 4870 – 96.
or conical.
Annual Book of ASTM Standards, Vol 06.03.
3 6.6 Weighing Bottles, with ground glass stoppers, num-
Annual Book of ASTM Standards, Vol 05.02.
Annual Book of ASTM Standards, Vol 14.03. bered, 80 mm diameter by 40 mm.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4870–99
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 Normal Heptane, ASTM knock test grade, conforming
to the requirements of Specification D 2880.
NOTE 1—Warning: Flammable, vapor harmful if inhaled. See A1.1.
7.2 Toluene, conforming to Specification D 362.
NOTE 2—Warning: Flammable, vapor harmful. See A1.2.
7.3 Wash Solvent, consisting of 85 volume % n-heptane
FIG. 2 Arrangement of Filtration Apparatus
(7.1) and 15 volume % toluene (see 7.2).
6.7 Hotplate, electric.
8. Sampling
6.8 Steam Generator, to provide steam at 100 6 1°C.
8.1 Sample in accordance with Practice D 4057 or Practice
6.9 Vacuum Source, capable of providing the specified
D 4177.
vacuum.
6.10 Vacuum Gage, capable of measuring the specified
9. Procedure
vacuum.
6.11 Filter Medium, Whatman glass fiber filter medium, 9.1 Sample Preparation—Mix the whole sample, as re-
Grade GF/A, 47 mm diameter. ceived, thoroughly using a high speed mixer when practicable,
6.12 High Speed Mixer, any convenient type, minimum for 30 s. In all cases a sample taken on a glass or PTFE rod
speed 400 rpm. dipped to the bottom of the container must show a homoge-
6.13 Desiccator. neous appearance. For fuels with a high wax content (high pour
6.14 Cooling Vessel, a desiccator or other type of tightly point), or of very high viscosity, the sample must be heated
covered vessel for cooling the filter media before weighing. before stirring. The temperature must be either 15°C above the
The use of a drying agent is not recommended. pour point in the case of low viscosity fuels, or that equivalent
D4870–99
to 150 to 250 cSt in the case of high viscosity fuels. In no case cool the apparatus by passing tap water through the coils. Wash
should the temperature exceed 80°C. the filtration unit carefully with two portions of 25 6 1mLof
9.2 Filter Preparation—For each test, dry two filter media the wash solvent from a syringe or graduated wash bottle with
for 20 min in the oven at 110°C. Transfer each paper, a fine nozzle, taking care to remove any adhered sample from
separately, rapidly to a numbered weighing bottle and allow to the wall of the upper part of the apparatus. Carefully remove
cool in the cooling vessel to room temperature (5 to 10 min). the top portion of the filtration unit and wash the rim of the
Where two-pan balances are used, weigh each weighing bottle filter with a further 10 6 0.5 mL of the wash solvent in a
plus filter medium by the tare method against an empty similar similar manner. Finally wash the whole of the filter medium
bottle, to the nearest 0.001 g. area with 10 6 0.5 mL of n-heptane.
NOTE 3—Caution: The Whatman GF/A filter media are fragile and are NOTE 7—If the sample filters very rapidly, the vacuum should be
to be handled with care. Before use, check each medium for consistency, released before the first solvent washing, to ensure complete coverage of
and the possible presence of small defects (holes). the filter medium area by solvent. The vacuum should then be gently
reapplied for the subsequent operations.
NOTE 4—For convenience, it is useful to have a number of weighing
bottles dedicated to the procedure, the lightest of which is chosen as the
9.6 Apparatus Disassembly—After the filter medium ap-
tare. All weighing bottles should be stored in a desiccator in the vicinity
pears dry, discontinue the vacuum supply. Using the forceps,
of the balance. Do not place these weighing bottles in the oven since their
carefully remove each filter medium separately and transfer
weights are in equilibrium with the desiccant.
them to the oven at 110°C. Dry for 20 min and quickly transfer
9.3 Apparatus Assembly—Before use, check that the filter
them to the same numbered weighing bottles as used in 9.2.
support screen is clean. If necessary, the screen must be
Allow them to cool in the cooling vessel (6.13) to room
cleaned by boiling in a high boiling point aromatic solvent.
temperature (5 to 10 min) and reweigh them (against tare) to
When more than 2 % of the sinter area remains blocked by
the nearest 0.0001 g.
particulate matter after such cleaning, discard the screen and
10. Calculation
install a new one.
9.3.1 The filtration unit must be clean and dry before
10.1 Calculate the mass percentage of total sediment to the
assembly. Stack the two previously dried and weighed filter
nearest 0.01 % m/m using the following equation:
media on top of the sinter support with the mesh imprint side
~M 2 M ! 2 ~M 2 M !
5 4 3 2
down, using forceps, placing the one from the lower numbered S 5 (1)
10 M
weighing bottle on the bottom. Apply slight vacuum to aid in
centering the filter media, and place the top portion of the where:
filtration apparatus carefully on to the media before clamping. S = total sediment, % m/m,
M = mass of sample, g,
Shut off the vacuum and pass steam at 100 6 1°C through the
M = mass of lower filter medium before filtration, mg,
heating/cooling coils for 10 min prior to sample addition. 2
M = mass of lower filter medium after filtration, mg,
9.4 Sample Addition—Into a 30 mL beaker, pour approxi-
M = mass of upper filter medium before filtration, mg, and
mately 11 g of the fuel sample prepared as described in 9.1 and
M = mass of upper filter medium after filtration, mg.
weigh to the nearest 0.01 g. Connect the vacuum source and
apply vacuum to an absolute pressure of 40 6 2 kPa minimum
11. Report
(61.3 kPa vacuum). Heat the contents of the beaker to 100 6
11.1 Report the total sediment by hot filtration as the
2°C. Then transfer the contents at 100 6 2°C (Note 5) to the
average of duplicate determinations, to the nearest 0.01 %
center of the filter medium, taking care that no sample touches
m/m. If a 5-g sample has been used, report the results as total
the walls during transfer (Note 6). Reweigh the beaker to the
sediment (5 g) by hot filtration. If filtration is not complete
nearest 0.01 g. The quantity transferred should be 106 0.5 g.
within the specified 25 min, report the results as filtration time
When filtration is not complete in 25 min, discontinue the test
exceeds 25 min.
and repeat using 5 6 0.3 g of sample. If filtration is still not
11.2 Test Report—The test report shall contain at least the
complete in 25 min, report the result as filtration exceeds 25
following information:
min.
11.2.1 The type and identification of the product tested,
NOTE 5—It is expedient to weigh the beaker plus stirrer plus tempera-
11.2.2 A reference to this test method,
ture measurement device before and after transfer to avoid errors incurred
11.2.3 The result of the test (see 11.1),
by attempting to obtain a net weight. Any convenient means of heating the
11.2.4 Any deviation, by agreement or otherwise, from the
fuel sample to 1006 2°C may be used, such as hot plate, water or oil bath,
standard procedures specified (see 11.1), and
or an oven when equipped with a suitable stirrer. Samples that overheat
11.2.5 The date of the test.
above 105°C must be discarded and not reused.
NOTE 6—For samples of high viscosity or high sediment, level filtration 5
12. Precision and Bias
will be aided by small stage or even dropwise addition. It is preferable to
12.1 Precision—The precision of this test method as deter-
avoid 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 mined by the statistical examination of interlaboratory test
maintained for the 25-min period.
results is as follows:
9.5 Filter Washing—When the filtration is complete and the
upper filter medium appears dry, continue the steam and
The results of cooperative test programs, from which these values have been
vacuum for a further 5 min. Discontinue the steam supply and derived, can be obtained from ASTM Headquarters. Request RR: D02–1238.
D4870–99
12.1.1 Repeatability—The difference between successive different laboratories on nominally identical test material
test results, expressed as the average of duplicate determina- would, in the long run, in the normal and correct operation of
the test method, exceed the following values only one case in
tions, obtained by the same operator with the same apparatus
twenty:
under constant operating conditions on identical test material,
would, in the long run, in the normal and correct operation of
R 5 0.294=x for residual fuels, and (4)
the test method, exceed the following values only in one case
R 5 0.174 x for distillate fuels containing
=
in twenty:
residual components (5)
r 5 0.089 x for residual fuels, and (2)
=
where x = the average of the test results, % m/m.
12.2 Bias—Since there is no accepted reference material
r 5 0.048 x for distillate fuels containing
=
residual components (3) suitable for determining the bias for the procedure in this test
method, bias cannot be determined.
where x = the average of the test results, % m/m.
13. Keywords
12.1.2 Reproducibility—The difference between two test
results, expressed as the average of duplicate determinations 13.1 ageing; fuel oils; hot filtration; residual fuel; sediment;
independently obtained by different operators operating in storage stability; total sediment
ANNEX
(Mandatory Information)
A1. PRECAUTIONARY STATEMENTS
A1.1 n-Heptane A1.2 Toluene
Keep away from heat, sparks, and open flame. 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 OILS
(STANDARD PROCEDURES FOR AGEING)
X1.1 Scope X1.3 Summary of Test Method
X1.1.1 This test method describes two procedures for evalu- X1.3.1 Procedure A for Thermal Ageing—A sample of
ating the sediment forming tendency of residual fuel oils residual fuel oil is aged at 100°C for 24 h.
during storage.
X1.3.2 Procedure B for Chemical Ageing—A sample of
residual fuel oil is diluted with hexadecane (cetane) and then
NOTE X1.1—Experience has shown that this test method can be
heated to 100°C for 1 h.
applicable to other fuel oils as well, but precision is unknown and
additional testing is required to determine that precision. X1.3.3 Following ageing by the above p
...
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