ASTM D3605-00(2005)
(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
SIGNIFICANCE AND USE
Knowledge of the presence of trace metals in gas turbine fuels enables the user to predict performance and, when necessary, to take appropriate action to prevent corrosion.
SCOPE
1.1 This test method covers the determination of sodium, lead, calcium, and vanadium in Specification D 2880 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 values stated in 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.
General Information
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D3605–00 (Reapproved 2005)
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 D3605; 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 addedanalyteprovidesthecalibrationinformationnecessaryto
calculate the analyte content of the unaltered sample.
1.1 This test method covers the determination of sodium,
3.2 Lead is determined by atomic absorption in a premixed
lead, calcium, and vanadium in Specification D2880 Grade
air-acetylene flame, and sodium is determined by atomic
Nos. 1-GT and 2-GT fuels in the range from 0.1 to 2.0 mg/L.
absorption or atomic emission in a premixed air-acetylene
This test method is intended for the determination of oil-
flame. Calcium and vanadium are determined by atomic
soluble metals and not waterborne contaminants in oil-water
absorption or atomic emission in a premixed nitrous oxide-
mixtures.
acetylene flame.
1.2 The values stated in SI units are to be regarded as the
3.3 Most experience with this test method has been in the
standard.
atomic absorption mode, although flame emission has been
1.3 This standard does not purport to address all of the
used successfully. Details in the subsequent sections are
safety concerns, if any, associated with its use. It is the
written for the atomic absorption mode. If the flame emission
responsibility of the user of this standard to establish appro-
mode is used, minor details in the subsequent sections must be
priate safety and health practices and determine the applica-
altered to conform to standard practice for flame emission
bility of regulatory limitations prior to use.
spectroscopy. The precision statement applies only to the
2. Referenced Documents atomic absorption mode.
2.1 ASTM Standards:
NOTE 1—Some GT fuel users may wish to determine potassium in
D2880 Specification for Gas Turbine Fuel Oils
addition to other metals included in this method. Potassium can be
D4057 Practice for Manual Sampling of Petroleum and determined in a manner similar to that for sodium using a potassium
hollow cathode lamp, (unless flame emission mode is used) a wavelength
Petroleum Products
of 766.4 mm, and an appropriate organo-potassium standard. Precision
data for potassium have not been determined.
3. Summary of Test Method
3.1 The samples are prepared to conform with the require-
4. Significance and Use
ments of the method of standard additions, which is selected to
4.1 Knowledgeofthepresenceoftracemetalsingasturbine
obviate problems encountered with the direct analysis of
fuels enables the user to predict performance and, when
typical gas turbine fuels that exhibit significant variations in
necessary, to take appropriate action to prevent corrosion.
physical properties. Different, but known, amounts of analyte
are added to two portions of sample. These, together with the
5. Apparatus
unaltered sample, are burned in the flame of an atomic
5.1 Atomic Absorption Spectrophotometer, capable of mea-
absorption instrument that measures light absorption by the
suring radiation over the wavelength range from 280 to 600
atomized metals. The analysis of the sample portions with
nm. The instrument must be capable of measuring low-level
signals (approximately 1 % absorption or 0.004 absorbance
unit per mg/L vanadium). The instrument should also be
This test method is under the jurisdiction of ASTM Committee D02 on equipped as follows.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
5.1.1 Burner, with variable nebulizer and auxiliary oxidant
D02.03 on Elemental Analysis.
supply to reduce non-atomic absorption from unburned hydro-
Current edition approved May 1, 2005. Published May 2005. Originally
carbons which cause interferences.
approved in 1977. Last previous edition approved in 2000 as D3605 – 00. DOI:
10.1520/D3605-00R05.
5.1.1.1 Burner Head, capable of supporting a nitrous oxide-
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
acetylene flame.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
5.1.1.2 Burner Head, single- or multiple-slot, capable of
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. supporting an air-acetylene flame.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D3605–00 (2005)
TABLE 1 Experimental Conditions
5.1.2 Electronic Detection System, capable of reading to the
nearest 0.1 % absorption or 0.0004 absorbance. Element Mode Wavelength, nm Fuel Oxidant
5.1.2.1 The text describes the measurement of absorption Na Absorption 589.6 C H air
2 2
Na Emission 589.6 C H air
2 2
signals that is, either percent absorption or absorbance. For
Pb Absorption 283.3 C H air
2 2
instruments reading in percent absorption, absorption signals
Ca Absorption 422.7 C H N O
2 2 2
Ca Emission 422.7 C H N O
of 0.1 % absorption must be measurable. For instruments
2 2 2
V Absorption 318.34–318.40 C H N O
2 2 2
reading in absorbance, signals of 0.0004 absorbance must be
V Emission 437.9 C H N O
2 2 2
measurable.
5.1.3 Hollow Cathode Lamp Power Supply, regulated to
minimize drift.
6.3 OrganometallicStandards—Oil-solublesaltsofsodium,
5.1.4 Monochromator, capable of resolving the 318.34– lead, calcium, and vanadium of known concentration.
318.40-nm vanadium doublet from the 318.54-nm vanadium 6.4 Mixed Standard—Prepare a mixed standard containing
line. 250 mg/L each of sodium, lead, calcium, and vanadium by
dissolvingtheappropriateamountsoforganometallicstandards
5.1.5 Hollow Cathode Lamps, one each for calcium, so-
in 1,2,3,4-tetrahydronaphthalene and making the required di-
dium, lead, and vanadium.
lutions. Prepare fresh daily, as needed.
NOTE 2—Electrodeless-discharge lamps can be an acceptable alterna-
tive, but the precision of this method was determined with hollow cathode
7. Sampling
lamps.
7.1 Samples shall be taken in accordance with the instruc-
5.1.6 When the instrument has flame-emission capability, tions in Practice D4057.
the emission technique can be used for the analyses of sodium,
8. Procedure
calcium, and vanadium.
8.1 Fill two clean 25-mL volumetric flasks to the line with
5.2 Volumetric Flasks, 25-mL.
sample. With the microlitre syringe add 50 µL of mixed
5.3 Glass Vials, 40-mL, screw-cap type, polyethylene-lined
standard to one flask and 100 µLto the other. Touch the needle
caps.
of the syringe to the inner wall of the flask to ensure
5.4 Syringe, 100-µL, Hamilton type or equivalent.
quantitative transfer of the standard. Invert and mix the
contents.(Thetwoflasksarenowspikedwith0.5mg/Land1.0
6. Reagents
mg/L of sodium, lead, calcium, and vanadium). Alternatively,
weigh 25.0 g of sample into each of two clean disposable glass
6.1 Purity of Reagents—Reagent grade chemicals shall be
used in tests. Unless otherwise indicated, it is intended that all 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,
reagents conform to the specifications of the Committee on
Analytical Reagents of the American Chemical Society where calcium, and vanadium.)
8.2 Prepare a third spiked sample by adding approximately
such specifications are available. Other grades may be used,
provided it is ascertained that the reagent is of sufficiently high 1mLofthemixedstandardtoapproximately25mLofsample.
This solution serves only to aid in establishing satisfactory
purity to permit its use without lessening the accuracy of the
determination. operating conditions for the atomic absorption instrument.
8.3 Establish the atomic absorption instrument operating
6.2 1,2,3,4-tetrahydronaphthalene, practical grade,
conditions, which are recommended by the manufacturer, and
analyte-sterile.
consider the following special points. Select the mode, flame
NOTE 3—Analyte-sterile 1,2,3,4-tetrahydronaphthalene can be pre-
gases, and spectral lines from the information presented in
pared by extracting a portion of tetralin with an equal amount of
Table 1.
hydrochloric acid in a covered screw-cap vial. Heat the vial on a steam
8.4 Analysis:
bath for 1 h and shake the vial for 1 h. If the acid extracted 1,2,3,4-
8.4.1 Withtheatomicabsorptioninstrumentinoperationfor
tetrahydronaphthalene and unextracted 1,2,3,4-tetrahydronaphthalene
monitoring lead absorption and with 1,2,3,4-
give
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