ASTM D3605-00(2011)
(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 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 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 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D3605 − 00(Reapproved 2011)
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,
lead, calcium, and vanadium in Specification D2880 Grade 3.2 Lead is determined by atomic absorption in a premixed
Nos. 1-GT and 2-GT fuels in the range from 0.1 to 2.0 mg/L. air-acetylene flame, and sodium is determined by atomic
This test method is intended for the determination of oil- absorption or atomic emission in a premixed air-acetylene
soluble metals and not waterborne contaminants in oil-water flame. Calcium and vanadium are determined by atomic
mixtures. absorption or atomic emission in a premixed nitrous oxide-
acetylene flame.
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this 3.3 Most experience with this test method has been in the
standard. atomic absorption mode, although flame emission has been
used successfully. Details in the subsequent sections are
1.3 This standard does not purport to address all of the
written for the atomic absorption mode. If the flame emission
safety concerns, if any, associated with its use. It is the
mode is used, minor details in the subsequent sections must be
responsibility of the user of this standard to establish appro-
altered to conform to standard practice for flame emission
priate safety and health practices and determine the applica-
spectroscopy. The precision statement applies only to the
bility of regulatory limitations prior to use.
atomic absorption mode.
2. Referenced Documents
NOTE 1—Some GT fuel users may wish to determine potassium in
addition to other metals included in this method. Potassium can be
2.1 ASTM Standards:
determined in a manner similar to that for sodium using a potassium
D2880 Specification for Gas Turbine Fuel Oils
hollow cathode lamp, (unless flame emission mode is used) a wavelength
D4057 Practice for Manual Sampling of Petroleum and
of 766.4 mm, and an appropriate organo-potassium standard. Precision
Petroleum Products
data for potassium have not been determined.
3. Summary of Test Method
4. Significance and Use
3.1 The samples are prepared to conform with the require-
4.1 Knowledgeofthepresenceoftracemetalsingasturbine
ments of the method of standard additions, which is selected to
fuels enables the user to predict performance and, when
obviate problems encountered with the direct analysis of
necessary, to take appropriate action to prevent corrosion.
typical gas turbine fuels that exhibit significant variations in
physical properties. Different, but known, amounts of analyte
5. Apparatus
are added to two portions of sample. These, together with the
5.1 Atomic Absorption Spectrophotometer, capable of mea-
unaltered sample, are burned in the flame of an atomic
suring radiation over the wavelength range from 280 to 600
absorption instrument that measures light absorption by the
nm. The instrument must be capable of measuring low-level
atomized metals. The analysis of the sample portions with
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 Lubricantsand 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, 2011. Published May 2011. Originally
carbons which cause interferences.
approved in 1977. Last previous edition approved in 2005 as D3605 – 00 (2005).
DOI: 10.1520/D3605-00R11.
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 (2011)
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
Na Absorption 589.6 C H air
5.1.2.1 The text describes the measurement of absorption
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 Organometallic Standards—Oil-soluble salts of sodium,
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
5.1.5 Hollow Cathode Lamps, one each for calcium, so-
dissolvingtheappropriateamountsoforganometallicstandards
dium, lead, and vanadium.
in 1,2,3,4-tetrahydronaphthalene and making the required di-
NOTE 2—Electrodeless-discharge lamps can be an acceptable alterna-
lutions. Prepare fresh daily, as needed.
tive, but the precision of this method was determined with hollow cathode
lamps.
7. Sampling
5.1.6 When the instrument has flame-emission capability,
7.1 Samples shall be taken in accordance with the instruc-
the emission technique can be used for the analyses of sodium,
tions in Practice D4057.
calcium, and vanadium.
8. Procedure
5.2 Volumetric Flasks, 25-mL.
8.1 Fill two clean 25-mL volumetric flasks to the line with
5.3 Glass Vials, 40-mL, screw-cap type, polyethylene-lined
sample. With the microlitre syringe add 50 µL of mixed
caps.
standard to one flask and 100 µLto the other. Touch the needle
5.4 Syringe, 100-µL, Hamilton type or equivalent.
of the syringe to the inner wall of the flask to ensure
quantitative transfer of the standard. Invert and mix the
6. Reagents
contents.(Thetwoflasksarenowspikedwith0.5mg/Land1.0
mg/L of sodium, lead, calcium, and vanadium). Alternatively,
6.1 Purity of Reagents—Reagent grade chemicals shall be
weigh 25.0 g of sample into each of two clean disposable glass
used in tests. Unless otherwise indicated, it is intended that all
vials and add the standard in the same manner. (The two vials
reagents conform to the specifications of the Committee on
are now spiked with 0.5 mg/kg and 1.0 mg/kg of sodium, lead,
Analytical Reagents of the American Chemical Society where
calcium, and vanadium.)
such specifications are available. Other grades may be used,
provided it is ascertained that the reagent is of sufficiently high 8.2 Prepare a third spiked sample by adding approximately
purity to permit its use without lessening the accuracy of the 1mLofthemixedstandardtoapproximately25mLofsample.
determination. This solution serves only to aid in establishing satisfactory
operating conditions for the atomic absorption instrument.
6.2 1,2,3,4-tetrahydronaphthalene, practical grade, analyte-
8.3 Establish the atomic absorption instrument operating
sterile.
conditions, which are recommended by the manufacturer, and
NOTE3—Analyte-sterile1,2,3,4-tetrahydronaphthalenecanbeprepared
consider the following special points. Select the mode, flame
by extracting a portion of tetralin with an equal amount of hydrochloric
gases, and spectral lines from the information presented in
acid in a covered screw-cap vial. Heat the vial on a steam bath for1hand
Table 1.
shake the vial for 1 h. If the acid extracted 1,2,3,4-tetrahydronaphthalene
and unextracted 1,2,3,4-tetrahydronaphthalene give indistinguishable ab-
8.4 Analysis:
sorption signals for each of the analytes under optimal experimental
8.4.1 Withtheatomicabsorptioninstrumen
...
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