ASTM D5184-01(2006)
(Test Method)Standard Test Methods for Determination of Aluminum and Silicon in Fuel Oils by Ashing, Fusion, Inductively Coupled Plasma Atomic Emission Spectrometry, and Atomic Absorption Spectrometry
Standard Test Methods for Determination of Aluminum and Silicon in Fuel Oils by Ashing, Fusion, Inductively Coupled Plasma Atomic Emission Spectrometry, and Atomic Absorption Spectrometry
SIGNIFICANCE AND USE
Catalyst fines in fuel oils can cause abnormal engine wear. These test methods provide a means of determining silicon and aluminum, the major constituents of the catalysts.
SCOPE
1.1 These test methods cover the determination of aluminum and silicon in fuel oils at concentrations between 5 and 150 mg/kg for aluminum and 10 and 250 mg/kg for silicon.
1.2 Test Method A—Inductively coupled plasma atomic emission spectrometry is used in this test method to quantitatively determine aluminum and silicon.
1.3 Test Method B—Flame atomic absorption spectrometry is used in this test method to quantitatively determine aluminum and silicon.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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. Specific warning statements are given in Sections 7.6, 10.1, and 11.5.
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Designation: D5184 − 01(Reapproved 2006)
Standard Test Methods for
Determination of Aluminum and Silicon in Fuel Oils by
Ashing, Fusion, Inductively Coupled Plasma Atomic
Emission Spectrometry, and Atomic Absorption
Spectrometry
This standard is issued under the fixed designation D5184; 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 Measurement System Performance
E135 Terminology Relating to Analytical Chemistry for
1.1 These test methods cover the determination of alumi-
Metals, Ores, and Related Materials
num and silicon in fuel oils at concentrations between 5 and
150 mg/kg for aluminum and 10 and 250 mg/kg for silicon.
3. Terminology
1.2 Test Method A—Inductively coupled plasma atomic
3.1 Definitions:
emission spectrometry is used in this test method to quantita-
3.1.1 emission spectroscopy—Refer to Terminology E135.
tively determine aluminum and silicon.
1.3 Test Method B—Flame atomic absorption spectrometry 3.2 Definitions of Terms Specific to This Standard:
is used in this test method to quantitatively determine alumi-
3.2.1 calibration—the process by which the relationship
num and silicon.
between signal intensity and elemental concentration is deter-
mined for a specific element analysis.
1.4 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
3.2.2 check standard—in calibration, an artifact measured
standard.
periodically, the results of which typically are plotted on a
1.5 This standard does not purport to address all of the
control chart to evaluate the measurement process.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Methods
priate safety and health practices and determine the applica-
4.1 Aweighed quantity of homogenized sample is heated in
bility of regulatory limitations prior to use. Specific warning
a clean platinum dish, the combustible material is removed by
statements are given in Sections 7.6, 10.1, and 11.5.
burning and the carbon finally removed by heating in a muffle
2. Referenced Documents furnace at a temperature of 550 6 25°C. The residue is fused
with a lithium tetraborate/lithium fluoride flux. The fused
2.1 ASTM Standards:
mixture is digested in a solution of tartaric acid and hydrochlo-
D1193 Specification for Reagent Water
ric acid and diluted to volume with water. The resulting
D4057 Practice for Manual Sampling of Petroleum and
solution is aspirated into an inductively-coupled plasma and
Petroleum Products
the emission intensities of aluminum and silicon lines are
D4177 Practice for Automatic Sampling of Petroleum and
measured. Standard calibration solutions are also aspirated and
Petroleum Products
aluminum and silicon intensities are measured for comparison.
D6299 Practice for Applying Statistical Quality Assurance
Alternatively, the resulting solution is aspirated into the flame
and Control Charting Techniques to Evaluate Analytical
ofanatomicabsorptionspectrometerandtheabsorptionsofthe
resonance radiation of aluminum and silicon are measured.
These test methods are under the jurisdiction of ASTM Committee D02 on
Standard calibration solutions are also aspirated and aluminum
Petroleum Products and Lubricants and are the direct responsibility of Subcommit-
andsiliconabsorptionintensitiesaremeasuredforcomparison.
tee D02.03 on Elemental Analysis.
Current edition approved May 1, 2006. Published June 2006. Originally
approved in 1991. Last previous edition approved in 2001 as D5184 – 01. DOI:
5. Significance and Use
10.1520/D5184-01R06.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5.1 Catalyst fines in fuel oils can cause abnormal engine
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
wear. These test methods provide a means of determining
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. silicon and aluminum, the major constituents of the catalysts.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5184 − 01 (2006)
6. Apparatus 7.2 Purity of Water—Unless otherwise indicated, reference
towatershallbeunderstoodtomeanreagentwaterconforming
6.1 Balance, capable of weighing to 0.1 g, capacity of
to Type II of Specification D1193.
150 g.
7.3 Flux—Mixture of 90 % lithium tetraborate and 10 %
6.2 Choice of Instrument:
lithium fluoride.
6.2.1 Inductively-Coupled Plasma Atomic Emission
Spectrometer—Either a sequential or simultaneous spectrom-
NOTE 2—Lithium fluoride is necessary to prevent heavy metal corro-
eterissuitable,ifequippedwithanICPtorchandRFgenerator
sion of the platinum dish and to lower the fusion temperature.
to form and sustain the plasma.
7.4 Hydrochloric acid (36 % (m/m))—concentrated hydro-
6.2.2 Atomic Absorption Spectrometer—A suitable instru-
chloric acid.
ment will consist of modulated hollow cathode lamps or other
sources of resonance radiation of aluminum and silicon, a
7.5 Potassium Hydrogen Sulfate, fused solid.
nitrous oxide/acetylene burner, and a spectrometer with a
7.6 2-Propanol (Isopropyl Alcohol) (Warning—
suitable detection and read-out system.
Flammable; can be explosive when evaporated to or near
6.3 Homogenizer, non-aerating, high-speed shear mixer to
dryness.)
homogenize the sample.
7.7 Aqueous Standard Solutions .
NOTE 1—Ultrasonic bath and ultrasonic probe type homogenizers were
7.7.1 Aluminum Standard Solutions—Obtain a ready made,
not evaluated in the development of these test methods.
aqueous standard or prepare a standard from aluminum wire.
6.4 Electric Muffle Furnace, capable of being maintained at
7.7.1.1 Aluminum Solution (1000 mg/L)—Aqueous, ready
temperatures of 550 6 25°C and 925 6 25°C. The furnace
made commercial standard.
preferably having suitable apertures at front and rear to allow
a slow, natural draft of air to pass through. 7.7.1.2 Aluminum Solution (1000 mg/L)—Cut an arbitrary
length of 99.99 % minimum purity aluminum wire (2 mm
6.5 Electric Hot Plate, with or without magnetic stirring
diameteraluminumwirehasbeenfoundsatisfactory).Measure
capability.
the length to the nearest 0.1 cm and weigh the aluminum wire
6.6 Electric Oven, maintained at a temperature of 50 to
to the nearest 0.001 g. Determine the mass/cm for the alumi-
60°C.
num wire and cut a length of aluminum wire that is calculated
6.7 Graduated Cylinders, 10, 25, 50, and 100 mL. to be slightly greater than 1.000 g. Trim off the excess wire
until the mass is 1.000 6 0.005 g. Dissolve the aluminum wire
6.8 Pipettes, 1, 2, 5, 10, 20, and 25 mL.
in 50 mL of concentrated hydrochloric acid. Heat gently. Cool
6.9 Platinum Dish, 100 mL capacity, cleaned with fused
andtransferthesolutionto1000mLvolumetricflask.Diluteto
potassium hydrogen sulfate.
the mark with water.
6.10 Volumetric Flasks, 100 and 1000 mL.
7.7.2 Silicon Standard Solutions—Obtain a ready made,
aqueous standard or prepare a standard from silicon dioxide.
6.11 All glassware must be carefully cleaned with 1 + 1
7.7.2.1 Silicon Solution (1000 mg/L)—Aqueous, ready
hydrochloric acid and rinsed thoroughly with water to mini-
mize contamination.The use of chromic acid cleaning solution made commercial standard.
is not recommended.
7.7.2.2 Silicon Solution (1000 mg/L)—Using a zirconium
crucible with a close fitting lid, fuse 2.140 6 0.0107 g of
6.12 Zirconium crucible with close fitting zirconium lid, 30
silicon dioxide (99.99 % purity) with8gof sodium hydroxide
to 50 mL capacity.
until a clear melt is obtained. Cool and dissolve the melt in
100 mLofasolutionof1parthydrochloricacidbyvolumeand
7. Reagents
2 parts water by volume. Transfer this solution to a 1000 mL
7.1 Purity of Reagents—Reagent grade chemicals shall be
volumetric flask and dilute to the mark with water. Immedi-
used in all tests. Unless otherwise indicated, it is intended that
ately, transfer the contents of the flask to a plastic bottle.
all reagents conform to the specifications of the Committee on
Analytical Reagents of the American Chemical Society where
7.8 Tartaric Acid/Hydrochloric Acid Solution—Dissolve 5 g
such specifications are available. Other grades may be used,
of tartaric acid in about 500 mLof water acidified with 40 mL
provided it is first ascertained that the reagent is of sufficiently
of concentrated hydrochloric acid and dilute to 1000 mL with
high purity to permit its use without lessening the accuracy of
water.
the determination.
7.9 Toluene/2-Propanol Solution (1 + 1)—Mix one vol-
ume of toluene with one volume of 2-propanol.
7.10 Quality Control (QC) Samples, preferably are portions
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
of one or more liquid petroleum materials that are stable and
listed by the American Chemical Society, see Analar Standards for Laboratory
representative of the samples of interest. These QC samples
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
can be used to check the validity of the testing process as
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD. described in Section 18.
D5184 − 01 (2006)
8. Quality Control (QC) Sample Preparation 11.5 Remove the dish, cool the fusion melt to room tem-
perature and add 50 mL of the tartaric acid/hydrochloric acid
8.1 Preparation of QC Samples shall follow the same
solution. Place the dish and contents on the hot plate main-
protocol as defined for the test specimen (Sections 9, 10, and
tained at a temperature of approximately 80°C. Heat until the
11).
melt is dissolved. (Warning—Vaporization of a significant
amount of the liquid can lead to precipitation of an insoluble
9. Sampling
form of silica leading to erroneous results.)
9.1 The objective of sampling is to obtain a sample for
NOTE 5—Prolonged heating can be necessary to dissolve the melt
testing purposes that is representative of the entire quantity.
completely and obtain a solution.Agitation or the use of magnetic stirring
Thus, take samples in accordance with the instructions in
can be employed to speed dissolution of the melt.
Practice D4057 or D4177 . Typically, a gallon size container
11.6 Allow the solution to cool and then transfer it to a
filled to approximately three-fourths of capacity is satisfactory.
100-mL flask with water, washing the dish several times to
ensure transfer is complete. Make up to the mark with water.
10. Sample Handling
Then, transfer the solution to a plastic bottle.
10.1 Homogenization—It is extremely important to homog-
NOTE 6—Transferring the test solution to a plastic bottle is desirable
enize the fuel oil in the sample container in order to obtain a
becausethediluteacidsolutioncontainsfluoboricacidfromdissolutionof
representative specimen. (Warning—Failure to use this ho-
the flux. Storage tests have shown that there is no significant attack of
mogenization procedure can invalidate the results because
glasswareintheshortterm(uptooneweek),andthatthesolutiondoesnot
non-representative aliquots could be obtained and this could contain fluoride ion above the 5 mg/L concentration.
lead to erroneous results.)
12. Preparation of Calibration Solutions
10.2 Place the sample container in an oven at a temperature
12.1 Blank Solution—Prepare a blank solution containing
of 50 to 60°C. Keep the container in the oven until the sample
only 0.4 g flux and 50 mLof the tartaric acid/hydrochloric acid
comes to temperature. Insert the shaft of a high speed homog-
solution diluted to 100 mL. Transfer it to a plastic bottle.
enizer into the sample container so that the head of the shaft is
12.2 Aluminum—Prepare a 250 mg/L aluminum working
immersed to approximately 5 mm from the bottom of the
solution by diluting 25 mLof the 1000 mg/Lstandard solution
sample vessel. Mix the sample for about 5 min.
to100mLwithwater.Toeachoffourclean100mLvolumetric
flasks, add 0.4 g of flux and 50 mL of the tartaric acid/
11. Specimen Preparation
hydrochloric acid solution. To successive flasks add 2, 4, 10,
11.1 Weigh a clean platinum dish to the nearest 0.1 g.
and 20 mL of the 250 mg/L aluminum working solution and
Immediately transfer up to 50 g (but not less than 20 g) of the
dilute to 100 mL with water. The calibration solutions contain
well-mixed sample, preferably containing about 1.3 mg alumi-
5, 10, 25, and 50 mg/L of aluminum, respectively.
num, to the platinum dish and re-weigh the dish and contents
12.3 Silicon—Prepare a 250 mg/L silicon working solution
to the nearest 0.1 g to obtain the weight of the specimen.
by diluting 25 mL of 1000 mg/L standard solution to 100 mL
NOTE 3—The specimen mass proposed, based on the aluminum content
with water. To each of four clean 100 mL volumetric flasks,
will suffice for silicon as both elements are usually found in fuel oils at
add 0.4 g of flux and 50 mL of the tartaric acid/hydrochloric
similar concentrations.
acid solution. To successive flasks, add 2, 4, 10, and 20 mL of
11.2 Warmthedishandcontentsgentlywithabunsenflame
the 250 mg/L silicon working solution and dilute to 100 mL
until the sample can be ignited. Maintain the contents of the
with water. These calibration solutions contain 5, 10, 25, and
basin at a temperature such that most of the combustible
50 mg/L of silicon, respectively.
material is removed and only carbon and ash remain.
12.4 Transfer all calibration standards to plastic bottles.
NOTE 4—If the specimen contains considerable amounts of moisture,
NOTE 7—When both aluminum and silicon are being determined, the 5
foaming and frothing can cause loss of material. If this is the case, discard
to 50 mg/L calibration solutions can be combined providing there are no
the specimen and to a fresh portion add 1 to 2 mL of 2-propanol before
incompatibilityproblemscausedbythereagentsusedinthepreparationof
heating. If this is not satisfactory, add 10 mL of a mixture of equal parts
the standard solutions described in 7.7.1 and 7.7.2.
of toluene and 2-propanol and mix thoroughly. Place several strips of
ashlessfilterpaperinthemixtureandwarmgently.Whenthepaperbegins
TEST METHOD A—INDUCTIVELY-COUPLED
to burn, the greater part of the water will have been removed.
PLASMA ATOMIC EMISSION SPECTROMETRY
11.3 Place the dish and contents in a muffle furnace main-
13. Preparation of ICP Instrument
tained at a temperature of 550 6 25°C. Maintain the muffle
furnace at this tempe
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