Standard Test Method for Determination of Phosphorous in Nickel, Ferronickel, and Nickel Alloys by the Phosphovanadomolybdate Molecular Absorption Spectrometric Method

SIGNIFICANCE AND USE
This test method is used for the analysis of nickel, ferronickel, and nickel base alloy samples by molecular absorption spectrometry to check compliance with compositional specifications. It is assumed that all who use the procedure will be trained analysts capable of performing common laboratory procedures skillfully and safely. It is expected that the work will be performed in a properly equipped laboratory and that proper waste disposal procedures will be followed. Appropriate quality control practices must be followed, such as those described in Guide E 882.
SCOPE
1.1 This test method covers the determination of phosphorus in nickel, ferronickel, and nickel alloys in the 0.0007 % through 0.05 % range.
1.2 Arsenic, chromium, hafnium, niobium, silicon, tantalum, titanium, and tungsten interfere, but the interference can be avoided by complexation or volatilization (for Cr). The lowest phosphorus content (0.0007 %) can be reached only in samples with low contents of interfering elements.
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. For specific hazards associated with the use of this practice see Practices E 50. Refer to specific warning notes given throughout this test method.

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Status
Historical
Publication Date
09-Sep-2002
Current Stage
Ref Project

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ASTM E1917-02 - Standard Test Method for Determination of Phosphorous in Nickel, Ferronickel, and Nickel Alloys by the Phosphovanadomolybdate Molecular Absorption Spectrometric Method
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:E1917–02
Standard Test Method for
Determination of Phosphorus in Nickel, Ferronickel, and
Nickel Alloys by the Phosphovanadomolybdate Molecular
1
Absorption Spectrometric Method
This standard is issued under the fixed designation E 1917; 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 of Repeatability and Reproducibility for a Standard Test
3
Method by Inter-laboratory Tests
1.1 This test method covers the determination of phospho-
ISO 11400:1992(E) Nickel, Ferronickel and Nickel
rus in nickel, ferronickel, and nickel alloys in the 0.0007 %
Alloys—Determination of Phosphorus Content—
through 0.05 % range.
Phosphovanadomolybdate MolecularAbsorption Spectro-
1.2 Arsenic, chromium, hafnium, niobium, silicon, tanta-
3
metric Method
lum, titanium, and tungsten interfere, but the interference can
be avoided by complexation or volatilization (for Cr). The
3. Summary of Test Method
lowest phosphorus content (0.0007 %) can be reached only in
3.1 The sample is dissolved in a mixture of hydrochloric
samples with low contents of interfering elements.
acid and nitric acid. The solution is evaporated to perchloric
1.3 This standard does not purport to address all of the
acid fumes and chromium is removed as volatile chromyl
safety concerns, if any, associated with its use. It is the
chloride. Silicon and refractory elements are complexed with
responsibility of the user of this standard to establish appro-
fluoride ions. The phosphorus is converted to phosphovanado-
priate safety and health practices and determine the applica-
molybdic acid in a perchloric and nitric acid solution. The
bilityofregulatorylimitationspriortouse.Forspecifichazards
phosphovanadomolybdic acid is extracted with 2-methyl-2-
associated with the use of this practice see Practices E50.
pentanone in the presence of citric acid to complex arsenic.
Refer to specific warning notes given throughout this test
Absorbance is measured at 355 nm.
method.
4. Significance and Use
2. Referenced Documents
2 4.1 This test method is used for the analysis of nickel,
2.1 ASTM Standards:
ferronickel, and nickel base alloy samples by molecular ab-
E50 Practices for Apparatus, Reagents, and Safety Precau-
sorption spectrometry to check compliance with compositional
tions for Chemical Analysis of Metals
specifications. It is assumed that all who use the procedure will
E 882 Guide for Accountability and Quality Control in the
be trained analysts capable of performing common laboratory
Chemical Analysis Laboratory
procedures skillfully and safely. It is expected that the work
E 1452 Practice for Preparation of Calibration Solutions for
will be performed in a properly equipped laboratory and that
Spectrophotometric and for Spectroscopic Atomic Analy-
properwastedisposalprocedureswillbefollowed.Appropriate
sis
quality control practices must be followed, such as those
E 1601 Practice for Conducting Interlaboratory Study to
described in Guide E 882.
Evaluate the Performance of an Analytical Method
2.2 ISO Standards:
5. Apparatus
ISO 5725:1986 Precision of Test Methods—Determination
5.1 Spectrophotometer—Capable of measuring absorbance
at a wavelength of 355 nm.
1
5.2 Cells—To fit spectrophotometer, having an optical path
This practice is under the jurisdiction of ASTM Committee E01 on Analytical
Chemistry of Metals, Ores and Related Materials and is the direct responsibility of
of 1 cm.
Subcommittee E01.08 on Nickel, Cobalt and High Temperature Alloys.
Current edition approved Sept 10, 2002. Published June 2003. Originally NOTE 1—Cells having other dimensions can be used, provided suitable
approved in 1997. Last previous edition approved in 1997 as E 1917-97.
adjustments can be made in the amount of sample and reagents used.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on Available from American National Standards Institute, 11 West 42nd Street,
the ASTM website. New York, NY 10036.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

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E1917–02
5.3 Plastic separatory funnels, 250 mL capacity. 8.2 The laboratory sample is normally in the form of
millings or drillings and no further preparation of the sample is
necessary.
6. Reagents
8.3 If it is suspected that the laboratory sample is contami-
6.1 Purity and Concentration of Reagents—The purity and
nated
...

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