ASTM D6130-97a(2003)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D6130–97a (Reapproved 2003)
Standard Test Method for
Determination of Silicon and Other Elements in Engine
Coolant by Inductively Coupled Plasma-Atomic Emission
Spectroscopy
This standard is issued under the fixed designation D6130; 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 sion Spectrometric Method for Trace ElementAnalysis of
Water And Wastes, EPA-600/4-79-020, revised 1984
1.1 This test method covers the determination of silicon in
engine coolant by inductively coupled plasma-atomic emission
3. Summary of Test Method
spectroscopy (ICP-AES). Silicon can be determined as low as
3.1 Elements in solution are determined, either sequentially
the range of 5 ppm by this test method. Other elements also
or simultaneously, by ICP-AES. New or used engine coolants
found in engine coolant can be determined by this method.
are prepared by dilution. Samples and standards are introduced
Thistestmethodisapplicabletothedeterminationofdissolved
to the nebulizer using a peristaltic pump and the aerosol is
or dispersed elements.
injected into an argon-supported inductively coupled plasma.
1.2 This test method is applicable to both new and used
The high temperature of the plasma atomizes the sample and
engine coolant.
produces atomic emission intensities at wavelengths associated
1.3 The values stated in SI units are to be regarded as the
with the desired elements. Emission intensity is proportional to
standard.
concentration. Elemental determinations are made by compar-
1.4 This standard does not purport to address all of the
ing standard and sample emission intensities.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Significance and Use
priate safety and health practices and determine the applica-
4.1 Some engine coolants are formulated with silicon con-
bility of regulatory limitations prior to use.
taining additives. This test method provides a means of
determining the concentration of dissolved or dispersed ele-
2. Referenced Documents
2 ments which give an indication of this additive content in the
2.1 ASTM Standards:
3 engine coolant.
D1193 Specification for Reagent Water
D1176 Practice for Sampling and Preparing Aqueous Solu-
5. Interferences
tions of Engine Coolants orAntirusts for Testing Purposes
5.1 Interferences may be categorized as follows:
5.1.1 Spectral—Light emission from spectral sources other
E691 Practice for Conducting an Interlaboratory Study to
than the element of interest may contribute to apparent net
Determine the Precision of a Test Method
signal intensity. Sources of spectral interference include direct
2.2 US EPA Standards:
spectral line overlaps, broadened wings of intense spectral
Method 6010, Inductively Coupled Plasma Method, SW-
5 lines, ion-atom recombination continuum emission, molecular
846, Test Methods for Evaluating Solid Waste
band emission and stray (scattered) light from the emission of
Method 200.7, Inductively Coupled Plasma -Atomic Emis-
elements at high concentrations. Avoid overlaps by selecting
alternate analytical wavelengths.
5.1.2 Physical—Physical interferences are effects associ-
This test method is under the jurisdiction ofASTM Committee D15 on Engine
Coolants and is the direct responsibility of Subcommittee D15.04 on Chemical ated with sample nebulization and transport processes such as
Properties.
viscosity and particulate contamination.
Current edition approved Oct. 10, 1997. Published July 1998. Originally
5.1.3 Background—High background effects from scattered
published as D6130–97. Last previous edition D6130–97. DOI: 10.1520/D6130-
light, etc., can be compensated for by background correction
97AR03.
Annual Book of ASTM Standards, Vol 11.01.
adjacent to the analyte line.
Annual Book of ASTM Standards, Vol 15.05.
5.1.4 Chemical—Chemical interferences are caused by mo-
Annual Book of ASTM Standards, Vol 14.02.
lecular compound formation, ionization effects, and thermo-
Available from U. S. Environmental Protection Agency, Environmental Moni-
toring and Support Laboratory, Cincinnati, OH 45268. chemical effects associated with sample vaporization and
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D6130–97a (2003)
atomization in the plasma. Normally these effects are not instrument to equilibrate prior to signal integration. Water
pronounced and can be minimized by careful selection of should be run for an additional 60 s after standards containing
operating conditions (incident power, plasma observation po- boron. Calibration should be validated and stability of stan-
sition, etc.). dards should be monitored.
6. Apparatus 10. Sample Preparation
6.1 Spectrometer—Aninductivelycoupledplasmaemission 10.1 Dilute the sample with deionized water so the concen-
spectrometer of the simultaneous or sequential type including tration of the element(s) of interest is in the linear detection
1 1
RF generator, torch, nebulizer, spray chamber, recommended range of the instrument. Generally a ⁄20 or ⁄50 dilution for used
peristaltic pump and host computer. engine coolant and a ⁄100 dilution for engine coolant concen-
trate are sufficient. Samples may be prepared by weight to
7. Reagents and Materials
volume or by volume to volume. Be certain when preparing
7.1 PurityofChemicals—Reagentgradeorbetterchemicals dilutions by volume that the entire sample aliquot is trans-
ferred. Filter or centrifuge samples that contain particulate.
shall be used for preparation of all standards and samples.
Other grades may be used provided it is first ascertained that
11. Procedure
the reagent is of sufficiently high purity to permit its use
without lessen
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