ASTM D3605-00
(Test Method)Standard Test Method for Trace Metals in Gas Turbine Fuels by Atomic Absorption and Flame Emission Spectroscopy
Standard Test Method for Trace Metals in Gas Turbine Fuels by Atomic Absorption and Flame Emission Spectroscopy
SCOPE
1.1 This test method covers the determination of sodium, lead, calcium, and vanadium in Specification D2880 Grade Nos. 1-GT and 2-GT fuels in the range from 0.1 to 2.0 mg/L. This test method is intended for the determination of oil-soluble metals and not waterborne contaminants in oil-water mixtures.
1.2 The preferred units are milligrams per litre.
1.3 This standard does not purport to address all of the safety problems, 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.
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An American National Standard
Designation:D3605–00
Standard Test Method for
Trace Metals in Gas Turbine Fuels by Atomic Absorption
and Flame Emission Spectroscopy
This standard is issued under the fixed designation D 3605; 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.
1. Scope absorption or atomic emission in a premixed air-acetylene
flame. Calcium and vanadium are determined by atomic
1.1 This test method covers the determination of sodium,
absorption or atomic emission in a premixed nitrous oxide-
lead, calcium, and vanadium in Specification D 2880 Grade
acetylene flame.
Nos. 1-GT and 2-GT fuels in the range from 0.1 to 2.0 mg/L.
3.3 Most experience with this test method has been in the
This test method is intended for the determination of oil-
atomic absorption mode, although flame emission has been
soluble metals and not waterborne contaminants in oil-water
used successfully. Details in the subsequent sections are
mixtures.
written for the atomic absorption mode. If the flame emission
1.2 The preferred units are milligrams per litre.
mode is used, minor details in the subsequent sections must be
1.3 This standard does not purport to address all of the
altered to conform to standard practice for flame emission
safety concerns, if any, associated with its use. It is the
spectroscopy. The precision statement applies only to the
responsibility of the user of this standard to establish appro-
atomic absorption mode.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
NOTE 1—Some GT fuel users may wish to determine potassium in
addition to other metals included in this method. Potassium can be
2. Referenced Documents
determined in a manner similar to that for sodium using a potassium
hollow cathode lamp, (unless flame emission mode is used) a wavelength
2.1 ASTM Standards:
of 766.4 mm, and an appropriate organo-potassium standard. Precision
D 2880 Specification for Gas Turbine Fuel Oils
data for potassium have not been determined.
D 4057 Practice for Manual Sampling of Petroleum and
Petroleum Products
4. Significance and Use
4.1 Knowledgeofthepresenceoftracemetalsingasturbine
3. Summary of Test Method
fuels enables the user to predict performance and, when
3.1 The samples are prepared to conform with the require-
necessary, to take appropriate action to prevent corrosion.
ments of the method of standard additions, which is selected to
obviate problems encountered with the direct analysis of
5. Apparatus
typical gas turbine fuels that exhibit significant variations in
5.1 Atomic Absorption Spectrophotometer, capable of mea-
physical properties. Different, but known, amounts of analyte
suring radiation over the wavelength range from 280 to 600
are added to two portions of sample. These, together with the
nm. The instrument must be capable of measuring low-level
unaltered sample, are burned in the flame of an atomic
signals (approximately 1 % absorption or 0.004 absorbance
absorption instrument that measures light absorption by the
unit per mg/L vanadium). The instrument should also be
atomized metals. The analysis of the sample portions with
equipped as follows.
addedanalyteprovidesthecalibrationinformationnecessaryto
5.1.1 Burner, with variable nebulizer and auxiliary oxidant
calculate the analyte content of the unaltered sample.
supply to reduce nonatomic absorption from unburned hydro-
3.2 Lead is determined by atomic absorption in a premixed
carbons which cause interferences.
air-acetylene flame, and sodium is determined by atomic
5.1.1.1 Burner Head, capable of supporting a nitrous oxide-
acetylene flame.
1 5.1.1.2 Burner Head, single- or multiple-slot, capable of
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee supporting an air-acetylene flame.
D02.03 on Elemental Analysis.
5.1.2 Electronic Detection System, capable of reading to the
Current edition approved Aug. 10, 2000. Published August 2000. Originally
nearest 0.1 % absorption or 0.0004 absorbance.
e1
published as D 3605 – 77. Last previous edition D 3605 – 91 (1995) .
Annual Book of ASTM Standards, Vol 05.01.
Annual Book of ASTM Standards, Vol 05.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D3605–00
TABLE 1 Experimental Conditions
5.1.2.1 The text describes the measurement of absorption
signals that is, either percent absorption or absorbance. For Element Mode Wavelength, nm Fuel Oxidant
instruments reading in percent absorption, absorption signals
Na Absorption 589.6 C H air
2 2
Na Emission 589.6 C H air
of 0.1 % absorption must be measurable. For instruments 2 2
Pb Absorption 283.3 C H air
2 2
reading in absorbance, signals of 0.0004 absorbance must be
Ca Absorption 422.7 C H N O
2 2 2
measurable.
Ca Emission 422.7 C H N O
2 2 2
V Absorption 318.34–318.40 C H N O
2 2 2
5.1.3 Hollow Cathode Lamp Power Supply, regulated to
V Emission 437.9 C H N O
2 2 2
minimize drift.
5.1.4 Monochromator, capable of resolving the 318.34–
318.40-nm vanadium doublet from the 318.54-nm vanadium
6.3 OrganometallicStandards—Oil-solublesaltsofsodium,
line.
lead, calcium, and vanadium of known concentration.
5.1.5 Hollow Cathode Lamps, one each for calcium, so-
6.4 Mixed Standard—Prepare a mixed standard containing
dium, lead, and vanadium.
250 mg/L each of sodium, lead, calcium, and vanadium by
dissolvingtheappropriateamountsoforganometallicstandards
NOTE 2—Electrodeless-discharge lamps can be an acceptable alterna-
tive, but the precision of this method was determined with hollow cathode in 1,2,3,4-tetrahydronaphthalene and making the required di-
lamps.
lutions. Prepare fresh daily, as needed.
5.1.6 When the instrument has flame-emission capability,
7. Sampling
the emission technique can be used for the analyses of sodium,
7.1 Samples shall be taken in accordance with the instruc-
calcium, and vanadium.
tions in Practice D 4057.
5.2 Volumetric Flasks, 25-mL.
5.3 Glass Vials, 40-mL, screw-cap type, polyethylene-lined
8. Procedure
caps.
8.1 Fill two clean 25-mL volumetric flasks to the line with
5.4 Syringe, 100-µL, Hamilton type or equivalent.
sample. With the microlitre syringe add 50 µL of mixed
standard to one flask and 100 µLto the other. Touch the needle
6. Reagents
of the syringe to the inner wall of the flask to ensure
6.1 Purity of Reagents—Reagent grade chemicals shall be quantitative transfer of the standard. Invert and mix the
contents.(Thetwoflasksarenowspikedwith0.5mg/Land1.0
used in tests. Unless otherwise indicated, it is intended that all
reagents conform to the specifications of the Committee on mg/L of sodium, lead, calcium, and vanadium). Alternatively,
weigh 25.0 g of sample into each of two clean disposable glass
Analytical Reagents of the American Chemical Society where
such specifications are available. Other grades may be used, vials and add the standard in the same manner. (The two vials
are now spiked with 0.5 mg/kg and 1.0 mg/kg of sodium, lead,
provided it is ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the calcium, and vanadium.)
8.2 Prepare a third spiked sample by adding approximately
determination.
1mLofthemixedstandardtoapproximately25mLofsample.
6.2 1,2,3,4-tetrahydronaphthalene , practical grade,
This solution serves only to aid in establishing satisfactory
analyte-sterile.
operating conditions for the atomic absorption instrument.
NOTE 3—Analyte-sterile 1,2,3,4-tetrahydronaphthalene can be pre-
8.3 Establish the atomic absorption instrument operating
pared by extracting a portion of tetralin with an equal amount of
conditions, which are recommended by the manufacturer, and
hydrochloric acid in a covered screw-cap vial. Heat the vial on a steam
consider the following special points. Select the mode, flame
bath for 1 h and shake the vial for 1 h. If the acid extracted 1,2,3,4-
gases, and spectral lines from the information presented in
tetrahydronaphthalene and unextracted 1,2,3,4-tetrahydronaphthalene
give indistinguishable absorption signals for each of the analytes under Table 1.
optimal expe
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